Process for the preparation of isolated 3,4-diaminobenzenesulphonic acid

    公开(公告)号:US06787666B2

    公开(公告)日:2004-09-07

    申请号:US10663827

    申请日:2003-09-16

    IPC分类号: C07C30900

    CPC分类号: C07C303/06 C07C309/45

    摘要: Described herein is a process for the preparation of 3,4-diaminobenzenesulphonic acid, characterized in that 1,2-diaminobenzene is reacted with anhydrous sulphuric acid which optionally comprises SO3 in up to stoichiometric amount, at a temperature in the range from 100 to 160° C. with stirring for a reaction time of from 1 to 20 hours; water or ice is added to the reaction mixture, optionally with cooling, up to a sulphuric acid concentration in the range from 30 to 75% by weight, based on the total mixture; the 3,4-diaminobenzenesulphonic acid precipitated out of the reaction mixture is filtered off, optionally washed with dilute sulphuric acid and worked up.

    Process for preparing p-toluidine-2-sulphonic acid
    4.
    发明授权
    Process for preparing p-toluidine-2-sulphonic acid 失效
    对甲苯胺-2-磺酸的制备方法

    公开(公告)号:US4717514A

    公开(公告)日:1988-01-05

    申请号:US848357

    申请日:1986-04-04

    CPC分类号: C07C309/45

    摘要: P-Toluidine-2-sulphonic acid (5-amino-2-methylbenzenesulphonic acid) is obtained in very pure form and virtually free of p-toluidine-3-sulphonic acid (2-amino-5-methylbenzenesulphonic acid) by reacting p-toluidine at 10.degree.-55.degree. C. with oleum in sulphuric acid. The molar ratio of SO.sub.3 to p-toluidine in this reaction is 1-3.0:1. The reaction mixture is worked up by pouring into water and filtering off the precipitated p-toluidine-2-sulphonic acid.

    摘要翻译: 以非常纯的形式获得对甲苯胺-2-磺酸(5-氨基-2-甲基苯磺酸),实际上不含对甲苯胺-3-磺酸(2-氨基-5-甲基苯磺酸) 甲苯胺在10 -55℃下与发烟硫酸在硫酸中反应。 该反应中SO 3与对甲苯胺的摩尔比为1-3.0:1。 将反应混合物倒入水中并滤出沉淀的对甲苯胺-2-磺酸。

    Process for separating mixtures of nitrobenzaldehyde isomers
    8.
    发明授权
    Process for separating mixtures of nitrobenzaldehyde isomers 失效
    分离硝基苯甲醛异构体混合物的方法

    公开(公告)号:US5567854A

    公开(公告)日:1996-10-22

    申请号:US532513

    申请日:1995-09-22

    CPC分类号: C07C201/16

    摘要: 2- and 3-Nitrobenzaldehydes suitable for use as intermediates for the preparation of pharmaceuticals are obtained in a simple manner and without risk of uncontrolled decompositions by distilling mixtures of nitrobenzaldehyde isomers at bottom temperatures of at most 200.degree. C. in the presence of monomeric and/or polymeric aromatic amines and/or phenols and/or N- and S-containing phenothiazines.

    摘要翻译: 适用于制备药物的中间体的2-和3-硝基苯甲醛以简单的方式获得,没有不受控制的分解的风险,通过在最多200℃的底部温度下蒸馏硝基苯甲醛异构体的混合物,在单体和/ /或聚合芳族胺和/或酚类和/或含N-和S-的吩噻嗪。

    Process for the preparation of 5-fluoro-2-nitrobenzoic acid
    10.
    发明授权
    Process for the preparation of 5-fluoro-2-nitrobenzoic acid 失效
    5-氟-2-硝基苯甲酸的制备方法

    公开(公告)号:US5756831A

    公开(公告)日:1998-05-26

    申请号:US667833

    申请日:1996-06-20

    CPC分类号: C07C201/08

    摘要: 5-Fluoro-2-nitrobenzoic acid having low contents of 3-fluoro-2-nitro-benzoic acid is prepared in a simple manner by nitrating 3-fluorobenzoic acid in an anhydrous medium using an anhydrous nitrating acid and isolating and purifying 5-fluoro-2nitro-benzoic acid, by taking 7.5 to 15 parts by weight of water, based on 1 part by weight of 3-fluorobenzoic acid used, introducing the reaction mixture reacted to exhaustion into this volume of water taken, filtering off the precipitate formed and washing it with water.

    摘要翻译: 通过使用无水硝酸将氮氟酸在无水介质中硝化3-氟苯甲酸,分离纯化5-氟-2-硝基苯甲酸,得到3-氟-2-硝基 - 苯甲酸含量低的5-氟-2-硝基苯甲酸 -2-硝基 - 苯甲酸,通过使用7.5重量份水,以1重量份所用的3-氟苯甲酸为原料,将反应混合物反应至该体积的水中,滤出形成的沉淀物, 用水冲洗。