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1. 发明申请

WO9747590A3 PROCESS FOR THE PURIFICATION OF AN INTERMEDIATE IN THE PREPARATION OF IOPAMIDOL 审中-公开
标题翻译：在制备IOPAMIDOL过程中中间体的纯化方法
公开(公告)号：WO9747590A3
公开(公告)日：1998-04-02
申请号：PCT/EP9703021
申请日：1997-06-11
申请人： FRUCTAMINE SPA , DESANTIS NICOLA
发明人： DESANTIS NICOLA
IPC分类号： C07C231/02 , C07C231/24 , C07C237/46
CPC分类号： C07C231/24 , C07C231/02
摘要： This invention refers to a new process for the synthesis of (S)-N,N'-bis[(2-hydroxy-1-(hydroxy-methyl)ethyl]-5-[(2-hydroxy-1-oxopropyl]amino]-2,4,6-triiodo-1,3-benzendicarboxamide, of formula (III), starting from 5-amino-2,4,6-triiodo-1,3-benzendicarboxylic acid dichloride characterized by a new step of chromatographic purification through resins of (S)-5-[[2-(acetyloxy)-1-oxopropyl]amino]-2,4,6-triiodo-1,3-benzendicarboxylic acid dichloride, which enables the direct conversion to the compound of formula (III), without preventive isolation.
摘要翻译：本发明涉及合成（S）-N，N'-双[（2-羟基-1-（羟甲基）乙基] -5 - [（2-羟基-1-氧代丙基）氨基] - （III）的2,4,6-三碘-1,3-苯二甲酰胺，具有以下步骤的特征：（S）-5 - [[2- （乙酰氧基）-1-氧代丙基]氨基] -2,4,6-三碘-1,3-苯二甲酰二氯，其能够直接转化为式（III）化合物，而无需预防隔离。

2. 发明申请

WO1997047590A2 PROCESS FOR THE PURIFICATION OF AN INTERMEDIATE IN THE PREPARATION OF IOPAMIDOL 审中-公开
标题翻译：在制备IOPAMIDOL过程中中间体的纯化方法
公开(公告)号：WO1997047590A2
公开(公告)日：1997-12-18
申请号：PCT/EP1997003021
申请日：1997-06-11
申请人： FRUCTAMINE S.P.A. , DESANTIS, Nicola
发明人： FRUCTAMINE S.P.A.
IPC分类号： C07C231/02
CPC分类号： C07C231/24 , C07C231/02
摘要： This invention refers to a new process for the synthesis of (S)-N,N'-bis[(2-hydroxy-1-(hydroxy-methyl)ethyl]-5-[(2-hydroxy-1-oxopropyl]amino]-2,4,6-triiodo-1,3-benzendicarboxamide, of formula (III), starting from 5-amino-2,4,6-triiodo-1,3-benzendicarboxylic acid dichloride characterized by a new step of chromatographic purification through resins of (S)-5-[[2-(acetyloxy)-1-oxopropyl]amino]-2,4,6-triiodo-1,3-benzendicarboxylic acid dichloride, which enables the direct conversion to the compound of formula (III), without preventive isolation.
摘要翻译：本发明涉及合成（S）-N，N'-双[（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-1,3-苯二甲酰胺，由5-氨基-2,4,6-三碘-1,3-苯二甲酰氯开始，其特征在于新的色谱步骤通过（S）-5 - [[2-（乙酰氧基）-1-氧代丙基]氨基] -2,4,6-三碘-1,3-苯二甲酰二氯的树脂进行纯化，其能够直接转化为式（III），无预防隔离。

3. 发明申请

WO1998024755A1 PROCESS FOR THE PURIFICATION OF AN AMINOALCOHOL 审中-公开
标题翻译：用于净化氨基醇的方法
公开(公告)号：WO1998024755A1
公开(公告)日：1998-06-11
申请号：PCT/EP1997006725
申请日：1997-12-01
申请人： DIBRA S.P.A. , DESANTIS, Nicola , FEDELI, Franco
发明人： DIBRA S.P.A.
IPC分类号： C07C213/10
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).
摘要翻译：本发明涉及一种制备有机杂质含量低于0.1％，无机杂质低于0.05％的2-氨基-1,3-丙二醇的方法，包括以下步骤：a）形成2 - 氨基-1,3-丙二醇盐与酸反应; b）由步骤a）得到的盐与含有通式R-OH的醇的水溶液或水 - 有机混合物结晶，其中R是C1-C6直链或支链烷基链和（C3-C7）烷基溶纤剂基团的单（C1-C3）烷基醚; c）通过使用离子交换剂洗脱游离碱，得到所述碱的水溶液; d）固体2-氨基-1,3-丙二醇从步骤b）中定义的溶剂中沉淀或结晶。

4. 发明申请

WO1996037460A1 PROCESS FOR THE PREPARATION OF A DICARBOXYLIC ACID DICHLORIDE 审中-公开
标题翻译：制备二氯甲烷二氯化物的方法
公开(公告)号：WO1996037460A1
公开(公告)日：1996-11-28
申请号：PCT/EP1996002104
申请日：1996-05-17
申请人： FRUCTAMINE S.P.A. , MAURO, Marina , VISCARDI, Carlo, Felice , GATTI, Massimo , DESANTIS, Nicola
发明人： FRUCTAMINE S.P.A.
IPC分类号： C07C231/02
CPC分类号： C07C231/02
摘要： The present invention refers to a process for the preparation of S-(-)-5-[[2-(acetyloxy)-1-oxopropyl]-amino]-2,4,6-triiodo-1,3-benzenedicarboxylic acid dichloride of formula (I) comprising the reaction between S-(-)-[2-(acetyloxy)]propionic acid chloride and 5-amino-2,4,6-triiodo-1,3-benzenedicarboxylic acid dichloride, in an aprotic dipolar solvent and in presence of a halogenhydric acid.
摘要翻译：本发明涉及制备S - （ - ） - 5 - [[2-（乙酰氧基）-1-氧代丙基] - 氨基] -2,4,6-三碘-1,3-苯二甲酸二氯化物的方法包含S - （ - ） - [2-（乙酰氧基）]丙酰氯和5-氨基-2,4,6-三碘-1,3-苯二甲酸二氯化物之间的反应的式（I）的非质子偶极溶剂并在卤代羟酸的存在下进行。

5. 发明申请

WO9958494A3 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 审中-公开
标题翻译：制备S-N，N'-二[2-羟基-1-（羟基甲基）乙基] -5 - [（2-羟基-1-氧代 - 戊基） - 氨基] -2,4,6-三 1,3-苯二甲酰胺
公开(公告)号：WO9958494A3
公开(公告)日：2000-01-20
申请号：PCT/EP9902804
申请日：1999-04-26
申请人： BRACCO INT BV , DESANTIS NICOLA , INCANDELA SALVATORE
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'-双[2-羟基-1-（羟甲基）乙基] -5 - [（2-羟基-1-氧代丙基）氨基] -2,4,6-三碘代 - 包括形成S- N，N'-双[2-羟基-1（羟甲基）乙基] -5 - [（2-（乙酰氧基）-1-氧代丙基）氨基] -2,4 ，6-三碘-1,3-苯二甲酰胺，由S - （ - ） - 5 - [[2-（乙酰氧基）-1-氧代丙基]氨基] -2,4,6-三碘-1,3-苯二甲酸二氯化物和2-一种1,3-三丙二醇在溶剂中，其特征在于所述溶剂选自：低级醇，单烷基醚二醇和直链或支链环烷基醚。

6. 发明申请

WO1998034908A1 PROCESS FOR THE CRYSTALLIZATION FROM A LINEAR OR BRANCHED (C5-C6) ALCOHOL OR THEIR MIXTURES OF (S)-N,N'-bis[2-HYDROXY-1- (HYDROXYMETHYL)ETHYL]-5-[ (2-HYDROXY-1-OXOPROPYl)AMINO]-2,4,6- TRIIODO-1,3-BENZENDICARBOXAMIDE 审中-公开
标题翻译：由（S）-N，N'-双[2-羟基-1-（羟基甲基）乙基] -5 - [（2-羟基-2-甲氧基乙基）乙基）乙基]酯的（C5-C6）醇或其混合物的结晶的方法， 1-氧代壬基）氨基] -2,4,6-三硫代-1,3-苯二甲酰胺
公开(公告)号：WO1998034908A1
公开(公告)日：1998-08-13
申请号：PCT/IB1997000106
申请日：1997-02-11
申请人： BRACCO INTERNATIONAL B.V. , DESANTIS, Nicola
发明人： BRACCO INTERNATIONAL B.V.
IPC分类号： C07C231/22
CPC分类号： C07C231/22 , C07C237/46
摘要： Disclosed is a new process for the crystallisation of (S)-N,N'-bis[2-hydroxy-1- (hydroxymethyl)ethyl]-5-[ (2-hydroxy-1-oxopropyl)amino] -2,4,6-triiodo-1,3-benzendicarboxamide (I), using a linear or branched (C5-C6) alcohol or their mixtures.
摘要翻译：公开了（S）-N，N'-双[2-羟基-1-（羟甲基）乙基] -5 - [（2-羟基-1-氧代丙基）氨基] -2,4 ，6-三碘-1,3-苯二甲酰胺（I），使用直链或支链（C5-C6）醇或它们的混合物。

7. 发明申请

WO1998024757A1 A PROCESS FOR THE PREPARATION OF 5-AMINO-2,4,6-TRIIODO-1,3-BENZENEDICARBOXYLIC ACID DERIVATIVES 审中-公开
标题翻译：制备5-氨基-2,4,6-三硝基-1,3-苯二羧酸衍生物的方法
公开(公告)号：WO1998024757A1
公开(公告)日：1998-06-11
申请号：PCT/EP1997006720
申请日：1997-12-01
申请人： DIBRA S.P.A. , DESANTIS, Nicola
发明人： DIBRA S.P.A.
IPC分类号： C07C231/02
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 DEG 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.
摘要翻译：本发明涉及一种制备5-氨基-1,3-苯二甲酸的非离子碘化造影剂衍生物并在5-位具有羟基取代的酰氨基残基的方法，包括以下步骤，不分离任何中间体：a）使5-氨基-2,4,6-三碘-1,3-苯二甲酰氯与含有作为酯保护的羟基的酰氯反应，得到5-酰基氨基-2,4,6 三碘-1,3-苯二甲酰氯在二甲基乙酰胺中的溶液; b）将由步骤a）得到的粗溶液加入式NR1R2R3的叔胺，其中R1，R2，R3独立地为（C1-C12）直链或支链烷基，（C1-C3）烷基（C6-C10）芳基，（C1-C4）烯基，以酰氯的摩尔量为3-15％，保持反应温度在0〜30℃; c）将由步骤b）得到的溶液加入氨基醇中，得到相应的N，N'-双[2,4,6-三碘-1,3-苯二甲酰胺]，其直接水解以使保护的羟基脱保护。

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