Abstract: The present invention relates to the novel compound, 1,4,7,10-tetraazabicyclo[8.2.2]tetradecan-2-one of formula (I), its preparation and the use thereof for the preparation of tetraazamacrocycles.
Abstract: A process for the preparation of complexes of macrocyclic chelants with paramagnetic metal trivalent ions of formula (XII) ##STR1## wherein R.sub.1, R.sub.2 and Me.sup.3+ are as described in the following, comprising: a) reaction of 1,4,7,10-tetraazacyclododecane with triethyl orthoformate to give 5H,9bH-2a,4a,7,9a-octahydrotetraazacycloocta[cd]pentalene; b) carboxymethylation reaction in water; c) hydrolysis reaction in basic conditions; d) alkylation according to known methods with an epoxide in water; e) complexation according to known methods carried out in water by addition of a paramagnetic metal salt; f) purification by diafiltration, final desalting of the aqueous solution on ion exchange resins and g) crystallization or recovery.
Type:
Grant
Filed:
May 24, 1999
Date of Patent:
April 4, 2000
Assignee:
Dibra S.p.A.
Inventors:
Giorgio Ripa, Alessandro Scala, Marcella Murru, Carlo Felice Viscardi, Marina Ausonio, Chiara Scotti, Patrizia Cossutta
Abstract: A process for the preparation of complexes of macrocyclic chelants with paramagnetic metal trivalent ions of formula (XII) ##STR1## wherein R.sub.1, R.sub.2 and Me.sup.3+ are as described in the following, comprising: a) reaction of 1,4,7,10-tetraazacyclododecane with triethyl orthoformate to give 5H,9bH-2a,4a,7,9a-octahydrotetraazacycloocta[cd]pentalene; b) carboxymethylation reaction in water; c) hydrolysis reaction in basic conditions; d) alkylation according to known methods with an epoxide in water; e) complexation according to known methods carried out in water by addition of a paramagnetic metal salt; f) purification by diafiltration, final desalting of the aqueous solution on ion exchange resins and g) crystallization or recovery.
Type:
Grant
Filed:
May 24, 1999
Date of Patent:
March 28, 2000
Assignee:
Dibra S.p.A.
Inventors:
Giorgio Ripa, Alessandro Scala, Marcella Murru, Carlo Felice Viscardi, Marina Ausonio, Chiara Scotti, Patrizia Cossutta
Abstract: Devices, and a method for the use thereof, for the standardization of signal intensity in the formation of magnetic resonance images of the human body, said devices including one or more straight, bent or flexible closed tubes with an external diameter not greater than 3 cm, an internal diameter of not less than 0.2 cm and a length of not less than 8 cm, made of susbtantially diamagnetic material, other than glass, preferably a plastic material, particularly polyvinyl chloride, each of them being filled with aqueous solutions or gels containing paramagnetic components, said tubes being kept close to the body either by means of the positioning devices of the body to which they are fixed permanently or temporarily, or by fixings which, on one side, can be fixed to the human body and on the other keep the tubes in the required positior.
Type:
Grant
Filed:
February 19, 1997
Date of Patent:
February 29, 2000
Assignee:
Dibra S.p.A.
Inventors:
Angelo Gallotti, Christoph De Haen, Anne Marie Smith, Michael N. Eakins, Julius P. Zodda
Abstract: The present invention relates to the novel compound, 1,4,7,10-tetraazabicyclo[8.2.2]tetradecan-2-one of formula (I), its preparation and the use thereof for the preparation of tetraazamacrocycles and the mono and diacetic acid derivatives.
Abstract: The present invention relates to the novel compound, 1,4,7,10-tetraazabicyclo[8.2.2]tetradecan-2-one of formula (I), its preparation and the use thereof for the preparation of tetraazamacrocycles.
Abstract: A process for the preparation of tetraazamacro-cycles of general formula (I) ##STR1## wherein n, p and q can independently be 0 or 1, comprising the following steps:a): condensation of polyamines with a glyoxal derivative;b): condensation of the resulting compound with an alkylating agent;c): oxidation of the resulting compound with an oxidizing agent, to give a mixture of oxidated products which is submitted tod): hydrolysis in acid aqueous solution, to give the compound of formula (I).
Type:
Grant
Filed:
December 2, 1998
Date of Patent:
January 11, 2000
Assignee:
Dibra S.p.A.
Inventors:
Maria Argese, Giorgio Ripa, Alessandro Scala, Vittorio Valle
Abstract: A new class of branched dendrimeric macromolecules, is described essentially consisting of a polyvalent central nucleus and a series of polyoxaalkylene "dendra". Such molecules are characterized by the presence of at least one branch, attached either directly to the "core" or to a "dendron", which does not participate in the growth and which therefore differs from all the other functions of the macromolecule.
Abstract: The present invention relates to the novel compound, 1,4,7,10-tetraazabicyclo[8.2.2]tetradecan-2-one of formula (I), its preparation and the use thereof for the preparation of tetraazamacrocycles.
Abstract: A process for the preparation of 5-[acetyl(2,3-dihydroxypropyl)amino]-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-t riiodo-1,3-benzenedicarboxamide of formula (I), starting from 5-amino-1,3-benzenedicarboxylic acid of formula (II), comprising the following steps:step a) is the reaction in heterogeneous phase between 5-amino-2,4,6-triiodo-1,3-benzenedicarboxylic acid and thionyl chloride in a solvent selected from the group consisting of: straight or branched (C.sub.7 -C.sub.16) hydrocarbons, (C.sub.7 -C.sub.
Abstract: A process for the preparation of 1,4,7,10-tetraazacyclododecane-1,4,7-triacetic acid and the salts thereof of formula (I) ##STR1## which comprises the following steps: a) carboxymethylation reaction of a suitable precursor in water, with a haloacetic acid,b) hydrolysis reaction in basic conditions by addition of the base added at the previous step.
Type:
Grant
Filed:
June 10, 1998
Date of Patent:
October 5, 1999
Assignee:
Dibra S.p.A.
Inventors:
Giorgio Ripa, Alessandro Scala, Marcella Murru, Emanuela Panetta, Carlo Felice Viscardi, Marina Ausonio
Abstract: A process for the preparation of complexes of macrocyclic chelants with paramagnetic metal trivalent ions of formula (XII) ##STR1## wherein R.sub.1, R.sub.2 and Me.sup.3+ are as described in the following, comprising: a) reaction of 1,4,7,10-tetraazacyclododecane with triethyl orthoformate to give 5H,9bH-2a,4a,7,9a-octahydrotetraazacycloocta?cd!pentalene; b) carboxymethylation reaction in water; c) hydrolysis reaction in basic conditions; d) alkylation according to known methods with an epoxide in water; e) complexation according to known methods carried out in water by addition of a paramagnetic metal salt; f) purification by diafiltration, final desalting of the aqueous solution on ion exchange resins and g) crystallization or recovery.
Type:
Grant
Filed:
June 10, 1998
Date of Patent:
July 20, 1999
Assignee:
Dibra S.p.A.
Inventors:
Giorgio Ripa, Alessandro Scala, Marcella Murru, Carlo Felice Viscardi, Marina Ausonio, Chiara Scotti, Patrizia Cossutta
Abstract: A process for the preparation of 5H,9bH-2a,4a,7, 9a-octahydrotetraazacycloocta?cd!pentalene of formula (I) ##STR1## which comprises the reaction of 1,4,7,10-tetraazacyclododecane with triethyl orthoformate in the absence of solvent and in the presence of an acid catalyst.
Type:
Grant
Filed:
June 10, 1998
Date of Patent:
July 20, 1999
Assignee:
Dibra S.p.A.
Inventors:
Carlo Felice Viscardi, Marina Ausonio, Massimo Gagna, Carlo Secchi
Abstract: A process for the preparation of the compounds of formula (I), and (II) comprising the steps represented in the following Scheme, in which the substituents are as defined in the specification.
Type:
Grant
Filed:
July 23, 1998
Date of Patent:
July 13, 1999
Assignee:
Dibra S.p.A.
Inventors:
Marcella Murru, Emanuela Panetta, Fulvio Uberti, Andrea Beltrami, Giorgio Ripa
Abstract: Branched, dendrimeric macromolecules having a central nucleus and a series of polyoxaalkylene chains that radiate from the nucleus and spread into the surrounding space branching a cascade fashion until the desired size results. Molecules formed in this manner are free of excessive functional crowding on their outer surfaces. Synthetic methods of preparing these molecules and their uses are described.
Type:
Grant
Filed:
April 30, 1998
Date of Patent:
March 23, 1999
Assignee:
Dibra S.p.A.
Inventors:
Luigia Gozzini, Monica Muttoni, Christoph De Haen
Abstract: A process for the preparation of 1,4,7,10-tetraazacyclododecane of formula (I), starting from decahydro-2a,4a,6a,8a-tetraazacyclopent?fg!acenaphthylene of formula (II):comprising the direct step of hydrolysis in aqueous solution, in conditions of slightly acid, neutral or slightly basic pH, with a primary diamine of formula (V), in whichx ranges between 0 and 2, andQ is --CH.sub.2 CH(OH)CH.sub.2 --, --(CH.sub.2).sub.2 NH(CH.sub.2).sub.2 --, or --?(CH.sub.2).sub.2 NH!.sub.2 (CH.sub.2).sub.2, when x is 1, orQ is --CH.sub.2 -- when x is 2.
Abstract: A process for the preparation of tetraazamacrocycles of general formula (I) ##STR1## wherein n, p and q can independently be 0 or 1, comprising the following steps:a): condensation of polyamines with a glyoxal derivative;b): condensation of the resulting compound with an alkylating agent;c): oxidation of the resulting compound with an oxidizing agent, to give a mixture of oxidated products which is submitted tod): hydrolysis in acid aqueous solution, to give the compound of formula (I).
Type:
Grant
Filed:
June 19, 1997
Date of Patent:
March 9, 1999
Assignee:
Dibra S.p.A.
Inventors:
Maria Argese, Giorgio Ripa, Alessandro Scala, Vittorio Valle
Abstract: The present invention relates to a process for the preparation of 2-amino-1,3-propanediol, having a content of organic impurities lower than 0.1% and inorganic impurities lower than 0.05%, comprising the following steps:a) formation of a 2-amino-1,3-propanediol salt with an acid;b) crystallization of the salt resulting from step a) from an aqueous or a hydro-organic mixture with a solvent selected from the group consisting of an alcohol of general formula R--OH, wherein R is a C.sub.1 -C.sub.6 straight or branched alkyl chain, and a mono(C.sub.1 -C.sub.3)alkylether of the (C.sub.3 -C.sub.7)alkylcellosolve group;c) elution of the free base by using ion exchangers to give an aqueous solution of said base;d) precipitation or crystallization of the solid 2-amino-1,3-propanediol from a solvent as defined in step b).