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    • 7. 发明授权
    • Process for the purification of an aminoalcohol
    • 纯化氨基醇的方法
    • US5866719A
    • 1999-02-02
    • US984086
    • 1997-12-03
    • Nicola DesantisFranco Fedeli
    • Nicola DesantisFranco Fedeli
    • A61K49/04C07C213/02C07C213/10C07C215/10C07C231/02C07C237/46C07C213/00
    • C07C213/02C07C213/10
    • 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).
    • 本发明涉及一种制备2-氨基-1,3-丙二醇的方法,该方法的有机杂质含量低于0.1%,无机杂质低于0.05%,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)得到的盐与水溶液或水 - 有机混合物结晶,所述混合物与选自由通式R-OH组成的组的溶剂结合,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。
    • 8. 发明授权
    • Process for the preparation of
5-(acetyl(2,3-dihydroxypropyl)amino-N,N-bis(2,3-dihydroxypropyl)-2,4,6-t
riiodo
    • 制备5-(乙酰基(2,3-二羟基丙基)氨基-N,N-双(2,3-二羟基丙基)-2,4,6-三碘代
    • US5965772A
    • 1999-10-12
    • US84922
    • 1998-05-28
    • Nicola Desantis
    • Nicola Desantis
    • C07C233/00C07C229/62C07C231/02C07C231/08C07C233/33C07C237/46C07C237/52C07C233/05
    • C07C227/18C07C231/02C07C231/08C07C237/52
    • 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 (C.sub.7 -C.sub.16) hydrocarbons, (C.sub.7 -C.sub.8) 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.degree. C.
    • 制备式(5)的5- [乙酰基(2,3-二羟丙基)氨基] -N,N'-双(2,3-二羟基丙基)-2,4,6-三碘-1,3-苯二甲酰胺的方法, I),由式(II)的5-氨基-1,3-苯二甲酸开始,包括以下步骤:步骤a)是非均相中5-氨基-2,4,6-三碘-1 (C7-C16)烃,(C7-C8)芳香族烃,1,1,1-三氯乙烷,乙酸正丁酯,二甘醇二甲醚(二乙烯基醚)的溶剂中选择3-苯二甲酸和亚硫酰氯, 二乙二醇二甲醚),在催化量的叔胺的存在下,得到化合物(III); 步骤b)是化合物(III)与冰乙酸作为溶剂和试剂和亚硫酰氯的乙酰化反应; 步骤c)是通过化合物(IV)与1-氨基-2,3-丙二醇的反应,通过化合物(IV)在偶极非质子溶剂中的反应,形成化合物(V),所述偶极非质子溶剂选自二甲基甲酰胺 DMF),二甲基乙酰胺(DMA),二甲基亚砜(DMSO)或N-甲基 - 吡咯烷酮; 步骤d)是在碱性pH下,通过在40-90℃的温度下加入氢氧化钠 - 氢氧化钙混合物与3-氯-1,2-丙二醇或表氯醇,将化合物(Ⅴ)在水溶液中烷基化 DEG C.