公开(公告)号：EP1242638A1

公开(公告)日：2002-09-25

申请号：EP00985156.9

申请日：2000-12-11

申请人： DIBRA S.p.A.

发明人： DESANTIS, Nicola ,  INCANDELA, Salvatore

IPC分类号： C22B3/42 ,  C22B15/00 ,  C01B7/13 ,  C01B9/06 ,  C22B3/00

CPC分类号： C22B7/007 ,  C01B7/13 ,  C22B3/42 ,  C22B15/0084 ,  Y02P10/234 ,  Y02P10/236

摘要： The present invention relates to a process for recovering copper from solutions from the recovery of iodine from industrial wastes from the production of ionic and non-ionic iodinated X-ray contrast agents by use of chelating resins suitable for removing copper from aqueous solutions. The absorbed copper is displaced by treating the resins with a 10 % hydrochloric or sulfuric acid solution.

公开(公告)号：EP0973723A1

公开(公告)日：2000-01-26

申请号：EP98919198.6

申请日：1998-04-01

申请人： DIBRA S.p.A.

发明人： DESANTIS, Nicola

IPC分类号： C07C213/10 ,  C07C215/10

CPC分类号： C07C213/10 ,  C07C215/10

摘要： A process for the preparation of 3-amino-1,2-propanediol, commonly known as isoserinol, having an organic impurities content lower than 0.1 % and an inorganic impurities content lower than 0.05 %.

公开(公告)号：EP1242638B1

公开(公告)日：2003-11-19

申请号：EP00985156.9

申请日：2000-12-11

申请人： DIBRA S.p.A.

发明人： DESANTIS, Nicola ,  INCANDELA, Salvatore

IPC分类号： C22B3/42 ,  C22B15/00 ,  C01B7/13 ,  C01B9/06 ,  C22B3/00

CPC分类号： C22B7/007 ,  C01B7/13 ,  C22B3/42 ,  C22B15/0084 ,  Y02P10/234 ,  Y02P10/236

摘要： The present invention relates to a process for recovering copper from solutions from the recovery of iodine from industrial wastes from the production of ionic and non-ionic iodinated X-ray contrast agents by use of chelating resins suitable for removing copper from aqueous solutions. The absorbed copper is displaced by treating the resins with a 10 % hydrochloric or sulfuric acid solution.

公开(公告)号：EP0915835A1

公开(公告)日：1999-05-19

申请号：EP98928291.0

申请日：1998-05-19

申请人： BRACCO S.p.A. ,  DIBRA S.p.A.

发明人： DESANTIS, Nicola

IPC分类号： C07C233 ,  C07C231 ,  C07C237 ,  C07C229

CPC分类号： C07C227/18 ,  C07C231/02 ,  C07C231/08 ,  C07C237/52 ,  C07C233/33 ,  C07C229/62

摘要： A process for the preparation of 5-[acetyl (2,3-dihydroxypropyl)amino]-N,N'-bis (2,3-dihydroxypropyl)-2,4,6- triiodo-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 (C7-C16) hydrocarbons, (C7-C8) aromatic hydrocarbons, 1,1,1-trichloroethane, n-butyl acetate, diglyme (diethylene glycol dimethyl ether), in the presence of catalytic amounts of a tertiary amine, to give compound (III); step b) is the acetylation reaction of compound (III) with glacial acetic acid both as the solvent and the reagent and thionyl chloride; step c) is the formation of compound (V) by reaction of the compound (IV) with 1-amino-2,3-propanediol, by reaction of compound (IV) in a dipolar aprotic solvent, selected from the group of dimethylformamide (DMF), dimethylacetamide (DMA), dimethylsulfoxide (DMSO) or N-methyl-pyrrolidinone; step d) is the alkylation of the compound (V) in aqueous solution at basic pH, by addition of a sodium hydroxide-calcium hydroxide mixture, with 3-chloro-1,2-propanediol or epichlorohydrin, at a temperature of 40-90 °C.

公开(公告)号：EP0883597A1

公开(公告)日：1998-12-16

申请号：EP97952845.0

申请日：1997-12-01

申请人： DIBRA S.p.A.

发明人： DESANTIS, Nicola ,  FEDELI, Franco

IPC分类号： A61K49 ,  C07C213 ,  C07C215 ,  C07C231 ,  C07C237

CPC分类号： C07C213/02 ,  C07C213/10

摘要： 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 the general formula R-OH, wherein R is a C1-C6 straight or branched alkyl chain, and a mono (C1-C3)alkylether of the (C3-C7)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).

公开(公告)号：EP1075462A2

公开(公告)日：2001-02-14

申请号：EP99924824.8

申请日：1999-04-26

申请人： DIBRA S.p.A.

发明人： DESANTIS, Nicola ,  INCANDELA, Salvatore

IPC分类号： C07C231/02 ,  C07C231/18 ,  C07C237/46

CPC分类号： C07C231/02 ,  C07C231/18 ,  C07C237/46

摘要： A process for the preparation of S- N,N'- bis[2- hydroxy-1- (hydroxymethyl) ethyl]- 5-[(2- hydroxy-1- oxopropyl)amino]- 2,4,6- triiodo- 1,3- benzenedicarboxamide, comprising the formation of S- N,N'- bis[2- hydroxy- 1(hydroxymethyl)ethyl]- 5-[(2- (acetyloxy)- 1-oxopropyl)amino]- 2,4,6- triiodo-1,3- benzenedicarboxamide starting from S-(-)- 5-[[2- (acetyloxy)- 1-oxopropyl]amino]- 2,4,6- triiodo- 1,3- benzenedicarboxylic acid dichloride and 2- a mino-1,3- propanediol in a solvent, characterized in that the solvent is selected from the group consisting of: lower alcohols, monoalkyl ether glycols and straight or branched cyclic alkyl ethers.

摘要翻译： 制备S-N，N'-二[2-羟基-1-（羟基甲基）乙基] -5 - [（2-羟基-1-氧代丙基）氨基] -2,4,6-三碘 - 包括形成S-N，N'-双[2-羟基-1-（羟基甲基）乙基] -5 - [（2-（乙酰氧基）-1-氧代丙基）氨基] -2,4 - 苯并二甲酰胺 （ - ） - 5 - [[2-（乙酰氧基）-1-氧代丙基]氨基] -2,4,6-三碘代-1,3-苯二甲酰胺开始，由6-（三碘代-1,3-苯二甲酰胺） 和2-氨基-1,3-丙二醇的溶剂，其特征在于溶剂选自低级醇，单烷基醚二醇和直链或支链环状烷基醚。

公开(公告)号：EP0915835B1

公开(公告)日：2000-12-20

申请号：EP98928291.8

申请日：1998-05-19

申请人： BRACCO S.p.A. ,  DIBRA S.p.A.

发明人： DESANTIS, Nicola

IPC分类号： C07C237/52 ,  C07C231/08 ,  C07C231/02

CPC分类号： C07C227/18 ,  C07C231/02 ,  C07C231/08 ,  C07C237/52 ,  C07C233/33 ,  C07C229/62

摘要： A process for the preparation of 5-[acetyl (2,3-dihydroxypropyl)amino]-N,N'-bis (2,3-dihydroxypropyl)-2,4,6- triiodo-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 (C7-C16) hydrocarbons, (C7-C8) aromatic hydrocarbons, 1,1,1-trichloroethane, n-butyl acetate, diglyme (diethylene glycol dimethyl ether), in the presence of catalytic amounts of a tertiary amine, to give compound (III); step b) is the acetylation reaction of compound (III) with glacial acetic acid both as the solvent and the reagent and thionyl chloride; step c) is the formation of compound (V) by reaction of the compound (IV) with 1-amino-2,3-propanediol, by reaction of compound (IV) in a dipolar aprotic solvent, selected from the group of dimethylformamide (DMF), dimethylacetamide (DMA), dimethylsulfoxide (DMSO) or N-methyl-pyrrolidinone; step d) is the alkylation of the compound (V) in aqueous solution at basic pH, by addition of a sodium hydroxide-calcium hydroxide mixture, with 3-chloro-1,2-propanediol or epichlorohydrin, at a temperature of 40-90 °C.

公开(公告)号：EP0901460A1

公开(公告)日：1999-03-17

申请号：EP97952841.0

申请日：1997-12-01

申请人： DIBRA S.p.A.

发明人： DESANTIS, Nicola

IPC分类号： A61K49 ,  C07C231 ,  C07C237

CPC分类号： C07C231/02 ,  A61K49/0433 ,  C07B2200/07 ,  C07C237/46

摘要： The present invention relates to a process for the preparation of non-ionic iodinated contrast media derivatives of 5-amino-1,3-benzenedicarboxylic acid and having a hydroxy-substituted acylamino residue at the 5-position, comprising the following steps without isolating any intermediate: a) reacting 5-amino-2,4,6-triiodo-1,3-benzenedicarboxylic acid dichloride with an acyl chloride, containing hydroxy groups protected as ester, to give a solution of 5-acylamino-2,4,6-triiodo-1,3-benzenedicarboxylic acid dichloride in dimethylacetamide; b) adding the crude solution resulting from step a) with a tertiary amine of formula NR1R2R3, wherein R1, R2, R3 are independently a (C1-C12) straight or branched alkyl group, (C1-C3)alkyl(C6-C10)aryl group, (C1-C4)alkenyl group, in a 3-15 % amount on the basis of the molar amount of acyl chloride, keeping the reaction temperature between 0 and 30 °C; c) adding the solution resulting from step b) with an aminoalcohol to give the corresponding N,N'-bis[2,4,6-triiodo-1,3-benzenedicarboxamide] which is directly hydrolyzed to deprotect the protected hydroxy groups.