Abstract: This invention relates to solid crystalline forms of (1RS,3RS,6RS)-6-Dimethylaminomethyl-1-(3-methoxy-phenyl)cyclohexane-1,3-diol hydrochloride (1), methods of producing 1, methods of use of 1, use of 1 as analgesics and pharmaceutical compositions comprising 1.

Abstract: A process for the preparation of optically pure R (?) salbutamol of formula (6) and its pharmaceutically acceptable salts by using a (+) 4-nitro tartranilic acid as the resolving agent and a binary solvent system comprising alkyl acetate and C1 to C4 branched or normal chain alcohol for dissolution of the racemic mixture and resolving agent and purification of the 4-nitro tartranilic acid salt of R (?) salbutamol. 4-nitro tartranilic acid salt of R (?) salbutamol is converted into formic acid salt of R (?) 4-benzyl salbutamol followed by basification and debenzylation to form optically pure R (?) salbutamol. Optically pure (R)-salbutamol is obtained in good yield and high purity. The optically pure R (?) salbutamol is optionally converted into pharmaceutically acceptable salts.

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.

Abstract: The present invention relates to the purification of (2S,3S,5S)-5-amino-2-N,N-dibenzylamino-3-hydroxy-1,6-diphenylhexane (III) by making its crystalline acid addition salt, which can be used as such to produce Lopinavir/Ritonavir with high purity and yield.

Abstract: Objects of the present invention are to provide a purification process that enables Pd to be removed effectively, and to provide an electroluminescent material and an electroluminescent device obtained by employing the process. The present invention relates to a process for purifying an electroluminescent material, the process involving treating, with a phosphorus-containing material, an electroluminescent material that contains Pd as an impurity so as to remove the Pd.

Abstract: The present invention provides improved processes for the preparation of atomoxetine hydrochloride under reaction conditions that improve reaction yields and facilitate commercial synthesis. In particular, the invention is directed to the synthesis of atomoxetine HCl by adding HCl to a mixture of (R)-(?)-tomoxetine (S)-(+)-mandelate with an organic solvent, with or without a base and water.

Abstract: Compounds containing phenolic hydroxy groups are removed from a gas stream which contains at least one aromatic amine generated during the gas-phase hydrogenation reaction of the corresponding nitroaromatic compounds with hydrogen, by adsorption on a basic solid.

Abstract: A method for bisformylation an arylamine compound by reacting an arylamine compound with an alkyleneamine in a reaction mixture while refluxing an acid in the reaction mixture.

Abstract: The present invention describes a new process for obtainment of the cetamine enantiomers, from the racemic cetamine resolution with the aid of an agent of chiral resolution, which provides the selective crystallization of its enantiomers. The resolution agent is employed in special concentration conditions, which provides stability, reproducibility and high enantiomeric purity to the precipitated diasteromer salt, making feasible the industrial production of the S-cetamine and its pharmaceutically acceptable salts.

Abstract: Polyisocyanates of the diphenyl methane series having reduced color values are obtained by a) reacting aniline and formaldehyde in the presence of an acid catalyst to form a polyamine, b) neutralizing the reaction mixture containing polyamine with a base, c) separating the neutralized mixture into the aqueous and the organic phases, d) adding a base to the organic phase and then e) phosgenating the resulting polyamine to produce the corresponding polyisocyanate.

Abstract: Cis-Tramadol hydrochloride is prepared by forming a Mannich hydrochloride, liberating the Mannich base, reacting the Mannich base with a Grignard reagent to form a base hydrate of cis-Tramadol which is used to form pure cis-Tramadol hydrochloride. Also claimed is the base hydrate of cis-Tramadol per se and its use as a medicament.

Abstract: An improved synthesis of N,N,-disubstituted-p-phenylene-diamine (DSPDA) preferably di-n-butyl-p-phenylenediamine is disclosed. The improvement rests on the discovery that DSPDA and its salts are extremely sensitive to oxygen so that once the product DSPDA or its salt is formed, oxygen must be excluded from all manipulations.

Abstract: (R*,R*)-2-[(dimethylamino)methyl]-1-(3-methoxyphenyl)cyclohexanol (Tramadol) is synthesized in a Grignard reaction in the presence of an additive resulting in a higher trans:cis ratio of product than is obtained in the absence of the additive. The Grignard reaction between 3 bromoanisole and the appropriate Mannich base in the presence of an amine or ether additive gives the amine product in an improved trans/cis ratio. The base is converted to its hydrochloride and recrystallized from a low molecular weight nitrile such as acetonitrile until a greater than 98% trans/cis ratio is obtained. Recrystallization from isopropanol gives (R*,R*)2-[(dimethylamino)methyl]-1-(3-metboxyphenyl)cyclohexanol hydrochloride free of the nitrile solvent. A hydrochloride of Tramadol can be synthesized without increasing a ratio of trans:cis by including a step in which HCl is added to Tramadol base in the presence of toluene.

Abstract: This invention relates to stable aromatic amine compositions. These compositions comprise a) an organic compound containing at least one carboxylic acid group, and b) an aromatic amine. This invention also relates to a process for stabilizing the color of aromatic amines, and to the use of these aromatic amines as initiators for the preparation of polyether polyols.

Abstract: This invention relates to stable aromatic amine compositions. These compositions comprise a) an organic compound containing at least one carboxylic acid group,, and b) an aromatic amine. This invention also relates to a process for stabilizing the color of aromatic amines, and to the use of these aromatic amines as initiators for the preparation of polyether polyols.

Abstract: The invention provides a process for the recovery of ascorbic acid from a feed containing at least one precursor of ascorbic acid comprising converting the precursor into at least one product, the at least one product being ascorbic acid in an organic extractant composition, the organic extractant composition comprising at least one secondary or tertiary alkyl amine in which the aggregate number of carbon atoms is at least 20, as a primary extractant, and a polar extraction enhancer compound; wherein the extractant composition comprises at least 2 moles of the polar extraction enhancer compound per one mole of primary extractant; and subjecting the ascorbic acid-containing organic extractant composition to a stripping operation with aqueous solution at a temperature of at least 20° C. higher than the temperature at which the conversion is carried out; whereby there is obtained an aqueous solution of ascorbic acid in which the concentration of ascorbic acid is higher than 5%.

Abstract: The present invention relates to a phosphoric acid salt of N-methyl-o-phenylenediamine and processes for making the same. In preferred embodiments of the invention, the phosphoric acid salt of N-methyl-o-phenylenediamine has the general Formula I wherein n is a number between 0.5 and 1.0, between 0.7 and 0.8, or between 0.75 and 0.78. The process for making the phosphoric acid salt of N-methyl-o-phenylenediamine comprises (a) dissolving the N-methyl-o-phenylenediamine in a first solvent, and (b) reacting the dissolved N-methyl-o-phenylenediamine with crystalline phosphoric acid or phosphoric acid dissolved in a second solvent.

Abstract: A method of manufacture of 4-nitro-m-phenylenediamine sulfate is taught. The resultant compound is useful in the dyeing of keratinic fibers, particularly, human hair. It exhibits reduced toxicity and potential for damage to such fibers, and is easier to remove than are other known compounds.

Abstract: The invention concerns a new method for producing optically active 1-phenylethylamines, wherein (a) racemic 1-phenylethylamines are reacted with (S)-(-)-N-phenylcarbamate lactic acid in the presence of an aliphatic or aromatic hydrocarbon and in the presence of a lower aliphatic alcohol, wherein the reaction components are measured so that for every mole of racemic amine, between 0.25 and 0.5 mole of (S)-(-)-N-phenylcarbamate lactic acid are present, the reaction mixture is then concentrated at a liquid-phase temperature of up to 40.degree. C.

Abstract: This invention relates to stable aromatic amine compositions. These compositions comprise a) an organic compound containing at least one carboxylic acid group, and b) an aromatic amine. This invention also relates to a process for stabilizing the color of aromatic amines, and to the use of these aromatic amines as initiators for the preparation of polyether polyols.

Abstract: A process for purifying 1,3-bis(aminophenoxy benzene) (APB) on a manufacturing scale to at least 99.5% purity comprises the sequential steps of (a) forming the dihydrochloride salt of APB (hereinafter APB-HCl), (b) recrystallizing the APB-HCl from isopropyl alcohol, and (c) converting the APB-HCl to free APB.

Abstract: A method for the purification of dinitroanilines having herbicidal activity by means of the known reactions of denitrosation using acid, and denitration in a neutral or basic environment in the presence of a phase-transfer catalyst, wherein:the denitrosation reaction is effected on the dinitration mixture containing the dinitroaniline of interest and the corresponding unwanted N-nitroso- and N-dinitroaniline impurities, and in the absence of solvent,the denitration reaction is conducted sequentially to the denitrosation reaction in the same reactor with the addition to the denitrosation product as such of an aqueous base, and of the said phase-transfer catalyst.

Abstract: The disclosure is of a process for recovering valuable by-products of the condensation of phenol and a ketone from a mother liquor obtained for example upon crystallization of a 1:1 adduct of phenol and bisphenol, said mother liquor containing phenol, bisphenol, isomers, contaminant by-products of the condensation reaction of phenol with the ketone and acidic impurities. The mother liquor is distilled/evaporated leaving a tarry residue, which is the feedstock for the process of the invention. The recovery comprises heating the feedstock with proportions of an arylamine salt, to extract the bisphenol-A values as aminophenylhydroxylphenyl-alkanes.

Abstract: A process for the isolation and purification of (RR,SS)-2-?(dimethylamino)methyl!-1-(3-methoxyphenyl)cyclohexanol and its salts from a Grignard reaction mixture which includes the (RR,SS) isomer, the (RS,SR) isomer and Grignard reaction side products. An aqueous solution of HBr is added to the reaction mixture to effect the selective precipitation of the (RR,SS) hydrobromide isomer from the mixture while the (RS,SR) isomer remains in solution. The precipitated (RR,SS)-2-?(dimethylamino)methyl!-1-(3-methoxyphenyl)cyclohexanol hydrobromide is converted to (RR,SS)-2-?(dimethylamino)methyl!-1-(3-methoxyphenyl)cyclohexanol hydrochloride.

Abstract: The present invention concerns a process for producing crystals of 3-amino-2-hydroxyacetophenone salt having a high bulk density and improved flow properties, by treating 3-amino-2-hydroxyacetophenone of formula (1) ##STR1## or hydrogen halide salt thereof with sulfuric acid, in a solvent.

Abstract: The invention provides a process for the purification and isolation of (RR,SS)-2-dimethylaminomethyl-1-(3-methoxyphenyl)cyclohexanol from mixtures also containing the (RS,SR) isomer comprising reacting the above mixture in a solvent at elevated temperature under acidic conditions, whereby the (RS,SR) isomer is selectively converted to the (RR,SS) isomer, 1-(3-methoxyphenyl)-2-dimethylaminomethylcyclohex-6-ene, 1-(3-methoxyphenyl)-2-dimethyl-aminomethylcyclohex-1-ene or a mixture thereof, selectively precipitating the desired (RR,SS) isomer as an amine acid salt, and recrystallizing the purified product.

Abstract: A process for the improved purification and separation of trans 2-[(dimethylamino)methyl]-1-(3-methoxyphenyl)cyclohexanol hydrochloride from a reaction mixture containing the trans isomer, the cis isomer and Grignard reaction side products, comprising combining the mixture with a solution of hydrochloric acid in a low molecular weight alcohol or with gaseous hydrogen chloride in the presence of an organic solvent selected from medium molecular weight alcohols, ketones, esters and ethers or aromatic ethers, to effect the selective precipitation of trans 2-[(dimethylamino)methyl]-1-(3-methoxyphenyl)cyclohexanol hydrochloride.

Abstract: The invention relates to a process for working up to crystallization mother liquor which is obtained in the resolution of the racemate of 1-(4-chlorophenyl)-ethylamine of the formula (I) with S-(-)-N-phenylcarbamoyllactic acid of the formula (II) by removing the ethanol from the ethanolic crystallization mother liquor by distillation in a 1st step and stirring the residue which remains with tert.-butyl methyl ether or toluene in a second step and it being possible to employ the resulting crystalline salt of (R/S)-1-(4-chlorophenyl)-ethylamine and (S)-(-)-N-phenylcarbamoyllactic acid directly again for the resolution of the racemate. The (S)-form of the amine is mainly present in the mother liquor and can be racemised and added to the resolution of the racemate again.

Abstract: 3,5-Diaminobenzotrifluoride can be readily separated from 4-chloro-3,5-diaminobenzotrifluoride by the addition of hydrogen chloride. 3,5-Diaminobenzotrifluoride forms hydrochloride salt, while 4-chloro-3,5-diaminobenzotrifluoride does so much less readily.

Abstract: A process for the preparation of N,N-dimethyl-1-[1-(4-chlorophenyl)cyclobutyl]-3-methylbutylamine hydrochloride monohydrate, a non-hygroscopic material which can be used as a pharmaceutical in the treatment of depression.

Abstract: A process for the manufacture of ascorbic acid from 2-ketogulonic acid esters (KGAE) utilizing amine salts of the latter is disclosed.

Abstract: A Lewis acid contaminant is removed from a (hydrocarbylthio)aromatic amine by mixing a solid alkali metal hydroxide with a solution of the Lewis acid in the amine, preferably at about 110.degree.-120.degree. C., and then filtering the solids from the mixture.

Abstract: A method for removing residual cresidine from impure p-cresidine sulfonic acid which impure p-cresidine sulfonic acid contains from above two parts per billion to about 1500 parts per million of cresidine. The method comprises contacting an aqueous solution of the p-cresidine sulfonic acid with a sufficient quantity of particles of a crosslinked lipophilic porous resin for a sufficient time to reduce the concentration of p-cresidine in the cresidine sulfonic acid to less than 2 parts per billion.

Abstract: A process is disclosed for the separation of p-fluoroaniline from a mixture, containing aniline and p-fluoroaniline, by contacting the mixture with a mineral acid in the presence of an organic solvent. The corresponding salt of p-fluoro-aniline is insoluble and can easily be isolated by conventional means such as filtration. If desired, the isolated salt can be converted to p-fluoroaniline by reaction with a base.

Abstract: A process for purifying crude polyether polyols which are prepared by anionic polymerization of alkylene oxides in the presence of basic catalysts. The polyols are mixed with water and ortho-phosphoric acid in certain quantity ratios, an adsorption agent is incorporated in the reaction mixture, the mixture is filtered and the water is removed from the polyether polyol by distillation.

Abstract: A process of separating amines having different basicity constants is disclosed. The more reactive amine is converted to a salt which is extracted with water in a multiple stage countercurrent extractor. The salt form of the amine is converted to the free amine. In a preferred aspect of the invention the amine salt is an amine sulfite which can be converted to free amine and sulfur dioxide. The sulfur dioxide can be reused to generate more amine sulfite. The more reactive amine is then separated from the water and part of it recovered. The remainder of the more reactive amine is recycled to the countercurrent extractor. The less reactive amine is removed from the countercurrent extractor in the free amine state as an organic phase along with any organic solvent that is used. Part of the less reactive amine is recovered from the system while the remainder is converted to a salt and an aqueous solution thereof recycled to the countercurrent extractor.

Abstract: The purification of N-substituted aminobenzaldehydes, such as p-dimethylaminobenzaldehyde, is facilitated via the use of sequential suspension, acidification, solids removal, neutralization and product recovery steps.

Abstract: An acid extraction process for separating 3,4-dichloroaniline from 2,3-dichloroaniline and 2,5-dichloroaniline is disclosed. The process involves selectively forming 3,4-dichloroaniline hydrochloride, since it has a higher basicity than the other dichloroaniline isomers, in a multiple stage extraction unit. An aqueous solution of 3,4-dichloroaniline hydrochloride is removed from the multiple stage extraction unit and neutralized with a base to form an immiscible mixture of an aqueous salt solution and 3,4-dichloroaniline which are separated by decantation.

Abstract: A new process for the purification of photographic developer compounds using an anionic surfactant wherein unwanted impurities are removed either by being precipitated or dissolved.In this process the developer substance is freed from difficult to remove impurities.