首页> 外国专利> A process for preparing 5- (acetyl (2,3-dihydroxypropyl) amino) -N, N'-bis (2,3-dihydroxypropyl) -2,4,6-triiodo-1,3-benzenedicarboxamide.

A process for preparing 5- (acetyl (2,3-dihydroxypropyl) amino) -N, N'-bis (2,3-dihydroxypropyl) -2,4,6-triiodo-1,3-benzenedicarboxamide.

机译:一种制备5-(乙酰基(2,3-二羟丙基)氨基)-N,N′-双(2,3-二羟丙基)-2,4,6-三碘代-1,3-苯二甲酰胺的方法。

摘要

The present invention concerns a for preparing 5 [ACETYL (2,3 -DIHIDROXIPROPIL) AMINO] -N, N'-bis (2, 3-dihydroxypropyl) -2,4,6-triiodo-1,3 PROCESS -BENCENODICARBOXAMIDA represented by formula (I) FROM 5-amino-1,3-benzenedicarboxylic acid of formula (II). Said process comprising the steps: (a) REACTION IN PHASE BETWEEN Heterogeneous 5-amino-2,4,6-1,3-benzenedicarboxylic -TRIIODO and thionylchloride in a solvent selected from the group consisting of: HYDROCARBONS (C7-16) branched or straight chain, AROMATIC HYDROCARBONS (C7-8), 1,1,1-trichloroethane, n-butyl acetate, diglyme (diethylene glycol, dimethyl ether) in the presence of catalytic AMOUNTS OF A tERTIARY aMINE, to obtain a compound of formula (III); (B) acetylation reaction of said compound of formula (III) with glacial acetic acid, which acts both as a solvent and as reagent and THIONYL CHLORIDE; (C) forming a compound of formula (V) by reacting the compound of formula (IV) containing 1-amino -2.3 propanediol, by reacting the compound (IV) in a solvent selected from dipolar aprotic GROUP dimethylformamide (DMF), dimethylacetamide (DMA), dimethylsulfoxide (DMSO) ON -Methyl -pyrrolidine; (D) Alkylation OF SUCH COMPOUND (V) AQUEOUS SOLUTION TO A basic pH by addition of a mixture of calcium hydroxide and sodium hydroxide, WITH 3-chloro-propanediol or epichlorohydrin -1.2, and a temperature BETWEEN 40 AND 90 ° C.
机译:本发明涉及一种制备5 [乙酰基(2,3-二己基吡啶)氨基] -N,N′-双(2,3-二羟丙基)-2,4,6-三碘代-1,3的方法-BENCENODICARBOXAMIDA式(I)由式(II)的5-氨基-1,3-苯二甲酸形成。所述方法包括以下步骤:(a)在选自以下的溶剂中的非均相的5-氨基-2,4,6-1,3-苯二甲酸-TRIIODO和亚硫酰氯之间的反应:分支的烃(C7-16)或直链芳烃(C7-8),1,1,1-三氯乙烷,乙酸正丁酯,二甘醇二甲醚(二甘醇,二甲醚)在叔胺的催化下,得到下式的化合物(III); (B)上述式(Ⅲ)化合物与冰醋酸的乙酰化反应,该冰醋酸既起溶剂又起试剂的作用,并与亚硫酰氯反应; (C)通过使包含1-氨基-2.3丙二醇的式(IV)的化合物反应,通过使化合物(IV)在选自偶极非质子族GROUP DMF,DMF,二甲基乙酰胺的溶剂中反应来形成式(V)的化合物DMA),在-甲基-吡咯烷上的二甲基亚砜(DMSO); (D)将该化合物烷基化(V)通过加入氢氧化钙和氢氧化钠与3-氯丙二醇或环氧氯丙烷-1.2的混合物,在40至90°C的温度下将水溶液溶解至碱性pH。

著录项

  • 公开/公告号ES2152747T3

    专利类型

  • 公开/公告日2001-02-01

    原文格式PDF

  • 申请/专利权人 BRACCO S.P.A.;

    申请/专利号ES19980928291T

  • 发明设计人 DESANTIS NICOLA;

    申请日1998-05-19

  • 分类号C07C237/52;C07C231/08;C07C231/02;

  • 国家 ES

  • 入库时间 2022-08-22 01:22:23

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