Purification Or Recovery Patents (Class 564/216)
  • Patent number: 9242241
    Abstract: Aspects of the present invention relates to a copper containing Levyne molecular sieve having a silica to alumina mole ratio less than 30 and a Cu:Al atomic ratio less than 0.45, wherein the Levyne molecular sieve retains at least 60% of its surface area after exposure to a temperature of from about 750° C. to about 950° C. in the present of up to 10 volume percent water vapor for a time ranging from about 1 to about 48 hours.
    Type: Grant
    Filed: October 11, 2010
    Date of Patent: January 26, 2016
    Assignee: BASE SE
    Inventors: Ivor Bull, Ulrich Müller, Bilge Yilmaz
  • Publication number: 20140364649
    Abstract: Provided is a method for producing an optically active ceramide by an N-acylation (amidation) reaction of an optically active aminodiol, wherein a crude ceramide produced therein is purified by an industrially advantageous process. Namely, provided is a method for producing a high-purity ceramide that has high diastereo purity with high yield. A high-purity ceramide is produced by: a step wherein a ceramide represented by general formula (1) is produced by reacting an aminodiol with an alkyl ester having 1-5 carbon atoms of an aliphatic carboxylic acid having 12-24 carbon atoms, said aliphatic carboxylic acid optionally having a hydroxyl group, in a hydrocarbon solvent having 5-10 carbon atoms; and a step wherein an alcohol having 1-3 carbon atoms is added into the reaction mixture obtained in the preceding step, thereby causing crystals to precipitate.
    Type: Application
    Filed: November 7, 2012
    Publication date: December 11, 2014
    Applicant: TAKASAGO INTERNATIONAL CORPORATION
    Inventors: Kenya Ishida, Kenji Yagi
  • Publication number: 20140256984
    Abstract: The invention in some aspects relates to devices and methods for nucleating crystals under controlled conditions. In some aspects of the invention, devices and methods are provided for continuous crystallization.
    Type: Application
    Filed: February 6, 2014
    Publication date: September 11, 2014
    Applicant: Massachusetts Institute of Technology
    Inventors: Allan Stuart Myerson, Shin Yee Wong
  • Patent number: 8796446
    Abstract: A method of removing a carboxylic acid from a liquid including a tertiary amide solvent includes: forming an extraction medium including an acid-extracting tin species and an extraction solvent that is immiscible with the tertiary amide solvent; subsequently contacting the liquid with the extraction medium, forming a phase including a de-acidified tertiary amide solvent and a phase including the extraction solvent; and removing the phase including the extraction solvent, to afford a liquid including the de-acidified tertiary amide solvent. The acid-extracting tin species is one or more tin species obtained by reaction of a di(hydrocarbyl) tin oxide with less than one equivalent of a carboxylic acid, or tin species obtainable by reaction of a 1,3-diacyloxy-1,1,3,3-tetra-(hydrocarbyl)distannoxane with an aqueous base. A method of preparing a sucralose-6-acylate includes uses the foregoing method to remove a carboxylic acid from a liquid including a tertiary amide solvent and the sucralose-6-acylate.
    Type: Grant
    Filed: May 3, 2012
    Date of Patent: August 5, 2014
    Assignee: Tate & Lyle Technology Limited
    Inventors: David T. Coleman, Edward Micinski, James Edwin Wiley, Jr., Thomas A. Eilers, David A. Dentel
  • Patent number: 8722932
    Abstract: A method for separating a mixture of components by simulated moving bed chromatography: (1) feeding the simulated moving bed such that the eluting power of the liquid phase in the second zone is greater than that of the liquid phase in the third zone, trapping the target component inside the second and the third zone; (2) a solvent for dissolving the mixture to be separated, instead of the feeding solution, is fed into the simulated moving bed through the feeding port, and the eluting power of the liquid phase in the second zone is maintained greater than that of the liquid phase in the third zone, thereby both the pre-impurity and the post-impurity are rinsed off completely, and the target component trapped in the second and the third zone is further purified; and (3) the target component trapped in the simulated moving bed is rinsed off the bed.
    Type: Grant
    Filed: September 14, 2011
    Date of Patent: May 13, 2014
    Assignee: Ningbo Institute of Technology, Zhejiang University
    Inventor: Feng Wei
  • Publication number: 20140107328
    Abstract: Chemoselective isolation of aliphatic hydroxyl group-containing and aromatic hydroxyl group-containing compounds is accomplished via formation of polymeric siloxyl ethers. Chemoselective release of aliphatic hydroxyl group-containing and aromatic hydroxyl group-containing compounds from polymeric siloxyl reagents is described.
    Type: Application
    Filed: December 11, 2013
    Publication date: April 17, 2014
    Inventors: Erin E. CARLSON, Darci TRADER
  • Publication number: 20140088197
    Abstract: The present invention provides a mixed crystalline form VIII of agomelatine, its method of preparation, application and pharmaceutical composition. The said mixed crystal consists mainly of crystalline form VI of agomelatine. The said mixed crystalline form is stable and has good reproducibility. Through stability tests, it has been found to be superior to the crystalline form VI in terms of stability. As a result, the crystalline form VIII of the present invention possesses advantages in pharmaceutical preparation.
    Type: Application
    Filed: March 22, 2012
    Publication date: March 27, 2014
    Applicant: LES LABORATORIES SERVIER
    Inventors: Yu Huang, QING Long, Xueyan Zhu, Hanbin Shan, Zhedong Yuan, Xiong Yu
  • Patent number: 8664441
    Abstract: The compound of formula (I) is a water-stable, long acting ?2-selective adrenoceptor agonist useful as a bronchodilator in the treatment of bronchoconstriction associated with reversible obstructive airways diseases and the like. Processes for making the compound of formula (I), as well as related intermediates, are disclosed.
    Type: Grant
    Filed: July 3, 2013
    Date of Patent: March 4, 2014
    Assignee: Sunovion Pharmaceuticals Inc.
    Inventors: Craig R. Abolin, H. Scott Wilkinson, Paul McGlynn, William K. McVicar
  • Patent number: 8501994
    Abstract: The compound of formula (I) is a water-stable, long acting ?2-selective adrenoceptor agonist useful as a bronchodilator in the treatment of bronchoconstriction associated with reversible obstructive airways diseases and the like.
    Type: Grant
    Filed: August 22, 2008
    Date of Patent: August 6, 2013
    Assignee: Sunovion Pharmaceuticals Inc.
    Inventors: Craig R. Abolin, H. Scott Wilkinson, Paul McGlynn, William K. McVicar
  • Publication number: 20130090459
    Abstract: The present invention relates to methods for rapid crystallization of amino acids, drug molecules, proteins and DNA/peptides. One method for rapid crystallization of functional group-containing molecules selected from the group consisting of amino acids, drug molecules, proteins and DNA/peptides includes (A) providing at least one metal or metal oxide in particulate or thin film form to provide (a) selective nucleation sites for crystallization of the functional group-containing molecules due to interactions of their functional groups and metal surfaces or engineered metal surfaces and (b) a microwave-transparent medium to create a thermal gradient between the metal surfaces or engineered metal surfaces and a warmer solution containing functional group-containing molecules to be crystallized, and (B) conducting microwave heating to cause the functional group-containing molecules to be crystallized.
    Type: Application
    Filed: October 11, 2012
    Publication date: April 11, 2013
    Applicant: MORGAN STATE UNIVERSITY
    Inventor: Morgan State University
  • Publication number: 20120289693
    Abstract: A method of removing a carboxylic acid from a liquid including a tertiary amide solvent includes: A) forming an extraction medium including an acid-extracting tin species and an extraction solvent that is immiscible with the tertiary amide solvent; B) subsequently contacting the liquid with the extraction medium, forming a phase including a de-acidified tertiary amide solvent and a phase including the extraction solvent; and C) removing the phase including the extraction solvent, to afford a liquid including the de-acidified tertiary amide solvent. The acid-extracting tin species is one or more tin species obtainable by reaction of a di(hydrocarbyl)tin oxide with less than one equivalent of a carboxylic acid, tin species obtainable by reaction of a 1,3-diacyloxy-1,1,3,3-tetra-(hydrocarbyl)distannoxane with an aqueous base.
    Type: Application
    Filed: May 3, 2012
    Publication date: November 15, 2012
    Applicant: Tate & Lyle Technology Limited
    Inventors: David T. Coleman, Edward Micinski, James Edwin Wiley, JR., Thomas A. Eilers, David A. Dentel
  • Publication number: 20120252901
    Abstract: Agomelatine crystal, which is a drug for treating depression, and pharmaceutical compositions thereof are provided. The X-ray powder diffraction spectra of such agomelatine crystal, which is irradiated by Cu-K? and showed by 2?(degree), has characteristic diffraction peaks at 12.84, 13.84, 16.14, 18.56, 19.12, 20.86, 21.20, 23.84; its IR absorption pattern has characteristic absorption peaks at about 3234, 3060, 2940, 1638, 1511, 1436, 1249, 1215, 1184, 1032, 908, 828, 755, 588 cm-1, and its DSC endothermic transition temperature is 97.6° C. The use of the agomelatine crystal as an active ingredient in preparing a medicament for the treatment of depression is also provided.
    Type: Application
    Filed: December 13, 2010
    Publication date: October 4, 2012
    Applicant: TIANJIN TAIPU PHARMACEUTICAL SCIENCE & TECHNOLOGY DEVELOPMENT CO., LTD
    Inventors: Jianqiang Zhu, Qingson Tian, Jian Zhao
  • Publication number: 20120157675
    Abstract: A chlorinating agent such as a chloroiminium species is used to remove or neutralize tertiary acetamide present as a contaminant in a tertiary formamide solvent. Tertiary formamide solvent purified or treated in this manner can be used as a reaction vehicle for the chlorination of sucrose-6-acylates, thereby improving the yields of the desired sucralose-6-acylate (an intermediate in the production of sucralose).
    Type: Application
    Filed: June 18, 2010
    Publication date: June 21, 2012
    Applicant: Tate & Lyle Technology Limited
    Inventors: James Edwin Wiley, JR., Mohamad R. Jaber
  • Publication number: 20120071691
    Abstract: A method for separating a mixture of components by simulated moving bed chromatography: (1) feeding the simulated moving bed such that the eluting power of the liquid phase in the second zone is greater than that of the liquid phase in the third zone, trapping the target component inside the second and the third zone; (2) a solvent for dissolving the mixture to be separated, instead of the feeding solution, is fed into the simulated moving bed through the feeding port, and the eluting power of the liquid phase in the second zone is maintained greater than that of the liquid phase in the third zone, thereby both the pre-impurity and the post-impurity are rinsed off completely, and the target component trapped in the second and the third zone is further purified; and (3) the target component trapped in the simulated moving bed is rinsed off the bed.
    Type: Application
    Filed: September 14, 2011
    Publication date: March 22, 2012
    Applicant: NINGBO INSTITUTE OF TECHNOLOGY, ZHEJIANG UNIVERSITY
    Inventor: Feng WEI
  • Patent number: 8110706
    Abstract: A method of preparation of a highly pure salt of R,R-formoterol L-tartrate is disclosed. The process provides the most thermodynamically stable polymorph by recrystallization of a novel polymorph.
    Type: Grant
    Filed: April 26, 2010
    Date of Patent: February 7, 2012
    Assignee: Sunovion Pharmaceuticals Inc.
    Inventors: Gerald J. Tanoury, Chris H. Senanayake, Donald W. Kessler
  • Publication number: 20110305618
    Abstract: The invention pertains to a method for eluting a radionuclide-label or a radionuclide-labeled compound using a solid phase extraction resin, to a device for performing such a method, and to a computer program for controlling such a device.
    Type: Application
    Filed: December 12, 2009
    Publication date: December 15, 2011
    Applicant: BAYER SCHERING PHARMA AKTIENGESELLSCHAFT
    Inventors: Keith Graham, Axel Rother, Dominic Franck
  • Publication number: 20110266220
    Abstract: A method of separating components of mixtures of chemical compounds uses a nonporous membrane of copolymer of a perfluorinated cyclic or cyclizable monomer, and a 4 carbon dicarboxyl-containing comonomer, such as maleic anhydride. Optionally, the membrane composition includes an acyclic fluorinated olefin termonomer. The membranes provide a remarkably high selectivity of water relative to organic solvents and inorganic acids compared to dipolymer membranes of perfluorinated comonomers.
    Type: Application
    Filed: January 5, 2010
    Publication date: November 3, 2011
    Applicant: CMS TECHNOLOGIES HOLDINGS, INC.
    Inventors: Daniel Campos, Jonathan Lazzeri, Stuart M. Nemser
  • Publication number: 20110245510
    Abstract: A process for removing by-products from N-vinylamide-rich product mixtures (crude N-vinylamide), which comprises performing an extraction of the crude N-vinylamide with an organic solvent as the extractant.
    Type: Application
    Filed: November 12, 2009
    Publication date: October 6, 2011
    Applicant: BASF SE
    Inventors: Wolfgang Staffel, Regina Vogelsang, Roland Kessinger, Lembit Tuttelberg, Bernd Heida
  • Publication number: 20110175022
    Abstract: The present invention provides a method for preparing DMF for sucralose production, including, e.g., isolating DMF from a composition comprising DMF, water, and methanol, using a single-tower rectification system. In various embodiments of the present invention, the composition, after the removal of water and methanol, may be further dried/dehydrated, such as, by using a dehydration agent and/or filtration. The resulting substantially pure DMF may comprise at least about 98-99% DMF. The present invention further provides a method of preparing a composition comprising anhydrous sucrose for sucralose production, which may comprise mixing regular sucrose with a water-containing DMF composition, and drying the resulting sucrose-DMF composition. Also provided is a single-tower separation system for isolating DMF from a composition comprising DMF, water, and methanol.
    Type: Application
    Filed: October 21, 2010
    Publication date: July 21, 2011
    Inventors: David Losan Ho, Zhenghao Wan
  • Patent number: 7964753
    Abstract: A method of preparation of a highly pure salt of R,R-formoterol L-tartrate is disclosed. The process provides the most thermodynamically stable polymorph by recrystallization of a novel polymorph.
    Type: Grant
    Filed: June 7, 2010
    Date of Patent: June 21, 2011
    Assignee: Sunovion Pharmaceuticals Inc.
    Inventors: Gerald J. Tanoury, Chris H. Senanayake, Donald W. Kessler
  • Patent number: 7939566
    Abstract: Crystalline form III of the compound of formula (I): characterised by its powder X-ray diffraction diagram. Medicinal products containing the same which are useful in the treatment of melatoninergic disorders.
    Type: Grant
    Filed: November 10, 2009
    Date of Patent: May 10, 2011
    Assignee: Les Laboratoires Servier
    Inventors: Gerard Coquerel, Julie Linol, Jean-Claude Souvie
  • Publication number: 20100324159
    Abstract: Embodiments of the present invention are directed to porous resins for solid phase extractions. The resins feature at least one hydrophobic component, at least one hydrophilic component and at least one ion exchange functional group. The resins exhibit superior wetting and ion exchange performance.
    Type: Application
    Filed: August 12, 2010
    Publication date: December 23, 2010
    Applicant: Waters Technologies Corporation
    Inventors: Peter Jeng Jong LEE, John E. O'Gara
  • Publication number: 20100240927
    Abstract: The present invention relates to a new method for preparing micron-sized particles which comprises introducing in the particle formation vessel a solute solution in a solvent and a compressed fluid under supercritical conditions, wherein the vessel in which the particles are formed is at a pressure comprised between atmospheric pressure and 15 bar. The particles obtained present a small size, a limited size distribution, and low agglomeration. Particles with suitable fluidity can furthermore be prepared from products, for example, pharmaceutical active ingredients and/or excipients, with a low glass transition temperature.
    Type: Application
    Filed: October 16, 2008
    Publication date: September 23, 2010
    Applicant: ACTIVERY BIOTECH, SL
    Inventor: Andreas Kordikowdki
  • Patent number: 7732641
    Abstract: A method of preparation of a highly pure salt of R,R-formoterol L-tartrate is disclosed. The process provides the most thermodynamically stable polymorph by recrystallization of a novel polymorph.
    Type: Grant
    Filed: December 5, 2008
    Date of Patent: June 8, 2010
    Assignee: Sepracor Inc.
    Inventors: Gerald J. Tanoury, Chris H. Senanayake, Donald W. Kessler
  • Publication number: 20100016536
    Abstract: An improved process for separating and isolating individual polar protic monomer(s) and/or oligomer(s) on the basis of degree of polymerization. A liquid sample containing polar protic monomer(s) and/or oligomer(s) is introduced into a liquid chromatography (LC) column packed with a polar bonded stationary chromatographic phase. The individual polar protic monomer(s) and/or oligomer(s) are separated via a binary mobile phase elution. One or more individual fractions containing the monomer(s) and/or oligomer(s) are eluted. The polar protic monomer(s) and/or oligomer(s) may be proanthocyanidins, hydrolyzable tannins, oligosaccharides, oligonucleotides, peptides, acrylamides, polysorbates, polyketides, poloxarners, polyethylene glycols, polyoxyethylene alcohols or polyvinyl alcohols. The binary mobile phase comprises an A phase consisting essentially of a polar aprotic solvent and a B phase consisting essentially of a polar protic solvent. A process for separating and isolating xanthine(s) (e.g.
    Type: Application
    Filed: June 18, 2009
    Publication date: January 21, 2010
    Applicant: Mars, Inc
    Inventors: Mark A. Kelm, Christopher J. Johnson, Rebecca J. Robbins
  • Patent number: 7635721
    Abstract: Crystalline form III of the compound of formula (I): characterized by its powder X-ray diffraction diagram. Medicinal products containing the same which are useful in the treatment of melatoninergic disorders.
    Type: Grant
    Filed: August 2, 2006
    Date of Patent: December 22, 2009
    Assignee: Les Laboratoires Servier
    Inventors: Gerard Coquerel, Julie Linol, Jean-Claude Souvie
  • Patent number: 7547378
    Abstract: The invention relates to a process for distillatively purifying crude dimethylacetamide (crude DMAc) comprising DMAc, low boilers and high boilers 5 by removing the low boilers and the high boilers to obtain pure DMAc in one of the column configurations listed hereinbelow: (I) a main column (MC) with sidestream column (SC) or (II) a dividing wall column (DWC), which operating at least the main column (MC) in column configuration (I) and the dividing wall column (DWC) in column configuration (II) at a top pressure in the range from 0.5 to 1.8 bar absolute.
    Type: Grant
    Filed: April 5, 2004
    Date of Patent: June 16, 2009
    Assignee: BASF Aktiengesellschaft
    Inventors: Werner Peschel, Hartmut Schoenmakers, Klaus Althaus, Tanja Kirchner, Hartmut Staatz
  • Patent number: 7479572
    Abstract: A method of preparation of a highly pure salt of R,R-formoterol L-tartrate is disclosed. The process provides the most thermodynamically stable polymorph by recrystallization of a novel polymorph.
    Type: Grant
    Filed: January 14, 2008
    Date of Patent: January 20, 2009
    Assignee: Sepracor Inc.
    Inventors: Gerald J. Tanoury, Chris H. Senanayaka, Donald W. Kessler
  • Patent number: 7371890
    Abstract: A process for continuously preparing a compound which bears at least two functional groups which are each independently selected from the group consisting of nitrile group, carboxylic acid group, carboxylic ester group and carboxamide group.
    Type: Grant
    Filed: June 11, 2004
    Date of Patent: May 13, 2008
    Assignee: BASF Aktiengesellschaft
    Inventors: Wolfram Stüer, Jens Scheidel, Hartwig Voβ, Peter Baβler, Michael Röper
  • Patent number: 7342132
    Abstract: A method of preparation of a highly pure salt of R,R-formoterol L-tartrate is disclosed. The process provides the most thermodynamically stable polymorph by recrystallization of a novel polymorph.
    Type: Grant
    Filed: August 4, 2006
    Date of Patent: March 11, 2008
    Assignee: Sepracor Inc.
    Inventors: Gerald J. Tanoury, Chris H. Senanayake, Donald W. Kessler
  • Patent number: 7145036
    Abstract: A method of preparation of a highly pure salt of R,R-formoterol L-tartrate is disclosed. The process provides the most thermodynamically stable polymorph by recrystallization of a novel polymorph.
    Type: Grant
    Filed: February 7, 2005
    Date of Patent: December 5, 2006
    Assignee: Sepracor Inc.
    Inventors: Gerald J. Tanoury, Chris H. Senanayake, Donald W. Kessler
  • Patent number: 7002041
    Abstract: An amide composition containing an unsaturated amide, a sulfur-containing compound, and a weak acid salt. The composition can include an amide in crystalline form or the composition can be in form of aqueous solution. The composition can exhibit improved stability whereby polymerization of the amide is inhibited.
    Type: Grant
    Filed: November 4, 2002
    Date of Patent: February 21, 2006
    Assignee: Mitsui Chemicals, Inc.
    Inventors: Takeya Abe, Kenju Sasaki
  • Patent number: 6946060
    Abstract: A method to purify N,N-dimethylacetamide (DMAc) from an aqueous solution containing acetic acid as a contaminant. Two fractional distillation columns are arranged in a series. The solution containing the contaminant is provided to the first column with a temperature profile to result in acetic acid partitioning into the overhead water. The material remaining in the bottom portion of the first column is recycled to the first column and also provided into a second column, whereby DMAc free of acetic acid contamination is recovered, and remaining DMAc and acetic acid are returned to the first column for further separation. The method uses standard fractional distillation procedures and equipment, thus eliminating the need for more complex extractions and/or chromatographic separations.
    Type: Grant
    Filed: July 1, 2002
    Date of Patent: September 20, 2005
    Assignee: Mallinckrodt Inc.
    Inventor: Michael J. Gentilcore
  • Patent number: 6818792
    Abstract: Polymerizable compounds are prepared and/or worked up using at least one liquid ring pump by a process in which a working liquid which contains a material stream from the preparation and/or working-up of the polymerizable compound is used in a liquid ring pump.
    Type: Grant
    Filed: September 4, 2002
    Date of Patent: November 16, 2004
    Assignee: BASF Aktiengesellschaft
    Inventors: Gerhard Nestler, Jürgen Schröder, Nicole McGlone
  • Patent number: 6723877
    Abstract: A continuous process for the production of dimethylformamide comprising the steps: (a) reacting methyl formate and dimethylamine in a reactive distillation column under conditions to form dimethylformamide and by-product methanol; (b) vaporizing the by-product methanol and generating a liquid dimethylformamide while in said reactive distillation column; (c) removing at least a major portion of the by-product methanol as an overhead from said reactive distillation column; (d) removing a crude liquid dimethylformamide containing residual by-product methanol as a bottoms fraction from said reactive distillation column; (e) introducing said bottoms fraction containing dimethylformamide and residual by-product methanol to a purification column wherein the by-product methanol is removed from said dimethylformamide as an overhead and purified dimethylformamide is removed as a bottoms fraction; and, optionally, (f) recycling the by-product methanol removed as an overhead from the purification column to the reac
    Type: Grant
    Filed: June 16, 2003
    Date of Patent: April 20, 2004
    Assignee: Air Products and Chemicals, Inc.
    Inventors: Robin Joyce Maliszewskyj, Michael Gerard Turcotte, John William Mitchell
  • Patent number: 6720453
    Abstract: A method of preparation of a highly pure salt of R,R-formoterol L-tartrate is disclosed. The process provides the most thermodynamically stable polymorph by recrystallization of a novel polymorph.
    Type: Grant
    Filed: September 10, 2002
    Date of Patent: April 13, 2004
    Assignee: Sepracor Inc.
    Inventors: Gerald J. Tanoury, Chris H. Senanayake, Donald W Kessler
  • Publication number: 20040000470
    Abstract: A method to purify N,N-dimethylacetamide (DMAc) from an aqueous solution containing acetic acid as a contaminant. Two fractional distillation columns are arranged in a series. The solution containing the contaminant is provided to the first column with a temperature profile to result in acetic acid partitioning into the overhead water. The material remaining in the bottom portion of the first column is recycled to the first column and also provided into a second column, whereby DMAc free of acetic acid contamination is recovered, and remaining DMAc and acetic acid are returned to the first column for further separation. The method uses standard fractional distillation procedures and equipment, thus eliminating the need for more complex extractions and/or chromatographic separations.
    Type: Application
    Filed: July 1, 2002
    Publication date: January 1, 2004
    Applicant: MALLINCKRODT INC.
    Inventor: Michael J. Gentilcore
  • Patent number: 6537524
    Abstract: A medicament containing, separately or together, (A) formoterol or a pharmaceutically acceptable salt thereof or a solvate of formoterol or said salt and (B) a tiotropium salt of a pharmaceutically acceptable acid, for simultaneous, sequential or separate administration in the treatment of an inflammatory or obstructive airways disease.
    Type: Grant
    Filed: August 8, 2001
    Date of Patent: March 25, 2003
    Assignee: Novartis AG
    Inventors: Ian Francis Hassan, Jeremy Guy Clarke, Bernard Cuenoud
  • Patent number: 6489474
    Abstract: Object of the present invention is to provide a process for producing an amide compound with high efficiency by subjecting an oxime compound to Beckmann rearrangement in a liquid phase under mild reaction conditions. Namely, the invention relates to a process for producing an amide compound such as &egr;-caprolactam by subjecting an oxime compound such as cyclohexanone oxime to Beckmann rearrangement in a liquid phase, characterized in that the reaction is carried out in the presence of (1) a non-fluorine-containing sulfonic anhydride and an N,N-disubstituted amide compound or (2) at least one compound selected from the group consisting of sulfonic acids and anhydrides thereof, an N,N-disubstituted amide compound, and a carboxylic anhydride.
    Type: Grant
    Filed: December 21, 2001
    Date of Patent: December 3, 2002
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Yuuji Kawaragi, Tohru Setoyama
  • Patent number: 6472563
    Abstract: A method of preparation of a highly pure salt of R,R-formoterol L-tartrate is disclosed. The process provides the most thermodynamically stable polymorph by recrystallization of a novel polymorph.
    Type: Grant
    Filed: November 9, 2001
    Date of Patent: October 29, 2002
    Assignee: Sepracor Inc.
    Inventors: Gerald J. Tanoury, Chris H. Senanayake, Donald W Kessler
  • Patent number: 6465692
    Abstract: Formamide with low conductivity and a neutral or slightly basic pH is provided. Such formamide may be used in a sample loading solution for capillary electrophoretic separation of biomolecular analytes to enhance the efficiency of sample injection into the capillary and the intensity of the signal. Formamide of the present invention may be obtained by first purifying the formamide to a conductivity of below 7 micro mho, and then adjusting the pH of the purified formamide with a base to a range of about pH 6.5 to 7.5. The purification may be carried out by first removing the water from the formamide, and then distilling the dried formamide until the conductivity of formamide is below about 7 micro mho.
    Type: Grant
    Filed: December 22, 1999
    Date of Patent: October 15, 2002
    Assignee: Beckman Coulter, Inc.
    Inventors: M. Parameswara Reddy, Chitra K. Ratnayake, Yu Liu, Jirong Gu
  • Patent number: 6455715
    Abstract: A method is described for producing saturated dicarboxylic acids with a chain length of C6 to C21 or the corresponding diamidic dicarboxylic acids from fatty acid cleavage of unsaturated fatty acids or the bis-fatty acid diamides of these unsaturated fatty acids by oxidative ozonolysis and subsequent separation and purification of the dicarboxylic acids, whereby after oxidative ozonolysis, the reaction products are dissolved at a high temperature in a carboxylic acid or a mixture of several carboxylic acids with a medium chain length of C6 to C12 or esters of short-chain alcohols of these carboxylic acids as the recrystallization solvent.
    Type: Grant
    Filed: October 24, 2001
    Date of Patent: September 24, 2002
    Assignee: Dr. Frische GmbH
    Inventors: Rainer Frische, Katja Hegwein, Jürgen Volkheimer
  • Patent number: 6441234
    Abstract: In the process for preparing formamide by reaction of ammonia and carbon monoxide in the presence of at least one catalyst, sodium diformylamide is used as catalyst. If sodium methoxide is used as further active component, sodium diformylamide can be formed from this. In this process, sodium diformylamide is a particularly active and stable catalyst which can be recycled.
    Type: Grant
    Filed: July 17, 2001
    Date of Patent: August 27, 2002
    Assignee: Abbott Laboratories
    Inventors: Jürgen Dahlhaus, Jörn Karl, Michael Schulz, Anne Wenzel, Wolfgang Harder, Arthur Höhn
  • Patent number: 6417399
    Abstract: The present invention generally relates to the individual stereoisomers of the drug valnoctamide (a mixture of four stereoisomer kinds, VCD-valmethamide or 2-ethyl-3-methyl pentanamide) useful in treatment of neurological and psychotic disorders such as different kinds of epilepsy and affective disorders, and useful as tranquilizers and to treat pain, and to pharmaceutical compositions containing, as an active ingredient, these stereoisomers. The present invention further relates to a method for stereoselective separation and quantification of the four stereoisomers from a racemic mixture of VCD or plasma of patients treated with the racemic drug. The present invention further relates to a unique method for the synthesis of the individual stereoisomers.
    Type: Grant
    Filed: July 13, 1999
    Date of Patent: July 9, 2002
    Assignee: Yissum Research Development Company of the Hebrew University of Jerusalem
    Inventors: Meir Bialer, Boris Yagen, Ofer Spiegelstein, Michael Roeder, Volker Schurig
  • Patent number: 6268533
    Abstract: A method is disclosed for the preparation of optically pure isomers of formoterol by the reaction of an optically pure 4-benzyloxy-3-formamidostyrene oxide with an optically pure 4-methoxy-&agr;-methyl-N-(phenylmethyl)benzeneethanamine followed by debenzylation. Useful intermediates in the process are also disclosed, as are the novel L-tartrate salt of R,R-formoterol and pharmaceutical compositions thereof.
    Type: Grant
    Filed: January 27, 2000
    Date of Patent: July 31, 2001
    Assignee: Sepracor Inc.
    Inventors: Yun Gao, Robert Hett, Kevin Q. Fang, Stephen A. Wald, Chris Hugh Senanayake
  • Patent number: 6252112
    Abstract: A novel process for the preparation of (1S, 4R)- or (1R, 4S)-4-(2-amino-6-chloro-9H-purin-9-yl)-2 -cyclopentene-1-methanol of the formula is described.
    Type: Grant
    Filed: August 13, 1999
    Date of Patent: June 26, 2001
    Assignee: Lonza A.G.,
    Inventors: Christine Bernegger, Eva Maria Urban, Olwen Mary Birch, Kurt Burgdorf, Frank Brux, Kay-Sara Etter, Pierre Bossard, Walter Brieden, Laurent Duc, John Gordon, Colm O'Murchu, Yves Guggisberg
  • Patent number: 6072084
    Abstract: A highly polymerizable N-vinylcarboxylic acid amide having an N-1,3-butadienylcarboxylic acid amide content of 30 ppm or less, a process for producing the same, and a process for producing a homopolymer of N-vinylcarboxylic acid amide or a copolymer thereof with another copolymerizable monomer using the same. Also, a highly polymerizable N-vinylcarboxylic acid amide is produced by thermal cracking or catalytic cracking of N-(1-alkoxyethyl)carboxylic acid amide or ethylidenebiscarboxylic acid amide, wherein the N-vinylcarboxylic acid amide content of the N-(1-alkoxyethyl)carboxylic acid amide or ethylenebiscarboxylic acid amide is 10 wt % or less.
    Type: Grant
    Filed: December 2, 1998
    Date of Patent: June 6, 2000
    Assignee: Showa Denko K.K.
    Inventors: Toshiyuki Aizawa, Hitoshi Nakamura, Tetsuo Kudo, Kunitoshi Wakabayashi, Kenji Shimamura, Shun-ichi Nagamatsu
  • Patent number: 6033530
    Abstract: A process for the continuous distillation of thermolabile monomers under reduced pressure in a column includesfeeding the thermolabile monomers in vapor or liquid form to the column,introducing an inert distillation aid which forms a heteroazeotrope with the thermolabile monomers into the vaporizer at the bottom of the column, but separately from the monomer feed, and vaporizing into there or feeding an emulsion of thermolabile monomers and an inert distillation aid into the vaporizer or into the column,condensing the azeotrope at the top of the column and separating it in a phase separator, taking off the thermolabile monomers and returning the distillation aid to the column or, if desired, working it up by distillation andtaking off components having a higher boiling point than the thermolabile monomers from the bottom of the column.
    Type: Grant
    Filed: March 14, 1997
    Date of Patent: March 7, 2000
    Assignee: BASF Aktiengesellschaft
    Inventors: Manfred Winter, Jacques Dupuis
  • Patent number: 5981799
    Abstract: A method is provided for purifying a crude N-acetyl-para-aminophenol (APAP) containing color bodies or their precursors, the method comprising: a) forming a hot aqueous solution of the crude APAP; and b) subsequently contacting the hot solution with an acid washed adsorbent carbon, e.g., an activated carbon, which acid washed carbon, prior to such contact, has been pretreated by contacting it with an aqueous solution of a reducing sulfite.
    Type: Grant
    Filed: March 15, 1994
    Date of Patent: November 9, 1999
    Assignee: BASF Corporation
    Inventors: Olan Stanley Fruchey, Edward G. Zey, Larry O. Wheeler
  • Patent number: 5951828
    Abstract: In a process for the continuous distillation of thermolabile monomers under reduced pressure in the presence of formamide in a column,the thermolabile monomers are continuously fed in liquid form, separately from formamide, into the lower part of the column up to the middle of the column,Formamide is vaporized with a vaporizer at the bottom of the column and, together with constituents having higher boiling points than the thermolabile monomers, is discharged from the bottom of the column and replaced by addition of fresh formamide,the thermolabile monomers are taken off at a side offtake in the upper third of the column, with the distillation being controlled such that the monomers contain less than 5% by weight of formamide, anda product stream containing constituents which have a lower boiling point than the thermolabile monomers is taken off at the top of the column.
    Type: Grant
    Filed: March 14, 1997
    Date of Patent: September 14, 1999
    Assignee: BASF Aktiengesellschaft
    Inventors: Manfred Winter, Jacques Dupuis, Michael Kroner