Method for the production of 2,6-dichloro-5-fluoro-nicotinic acid and coarse and particularly pure 2,6-dichloro-5-fluoro-nicotinic acid
    4.
    发明授权
    Method for the production of 2,6-dichloro-5-fluoro-nicotinic acid and coarse and particularly pure 2,6-dichloro-5-fluoro-nicotinic acid 失效
    制备2,6-二氯-5-氟 - 烟酸的方法和粗的,特别纯的2,6-二氯-5-氟 - 烟酸

    公开(公告)号:US06441182B1

    公开(公告)日:2002-08-27

    申请号:US10009437

    申请日:2001-12-06

    IPC分类号: C07D21380

    CPC分类号: C07D213/80

    摘要: The invention relates to a method for the production of 2,6-dichloro-5-fluoronicotinic acid by hydrolyzing 2,6-dichloro-5-fluoro-3-cyanopyridine by (a) dissolving 2,6-dichloro-5-fluoro-3-cyanopyridine at 70 to 90° C. in sulfuric acid having a concentration of 90 to 99% by weight and hydrolyzing the 2,6-dichloro-5-fluoro-3-cyanopyridine at 70 to 100° C. to the corresponding carboxamide, (b) cooling the resultant reaction mixture to a temperature in the range from 10 to 65° C., (c) metering in water until the concentration of sulfuric acid is 55 to 75% by weight (calculated relative to the sulfuric acid employed in stage (a) and the water employed in stage (c)) while keeping the temperature between 30 and 65° C. during the addition of the first quarter of the water and keeping the temperature between 50 and 80° C. during the addition of the second quarter of the water, and (d) completing hydrolysis of the resultant mixture to 2,6-dichloro-5-fluoronicotinic acid at 70 to 110° C.

    摘要翻译: 本发明涉及通过(a)将2,6-二氯-5-氟-3-氰基吡啶溶解在2,6-二氯-5-氟-3-氰基吡啶中的方法制备2,6-二氯-5-氟烟酸, 在70〜90℃,在浓度为90〜99重量%的硫酸中,在70〜100℃下将2,6-二氯-5-氟-3-氰基吡啶水解成相应的羧酰胺 ,(b)将所得反应混合物冷却至10至65℃的温度,(c)在水中计量直到硫酸浓度为55至75重量%(相对于所用的硫酸计算) 在阶段(a)和阶段(c)中使用的水),同时在添加第一季度期间保持温度在30和65℃之间,并且在添加期间保持温度在50和80℃之间 的水,和(d)在70-110℃下将所得混合物完全水解成2,6-二氯-5-氟烟酸。

    Process for the preparation of dialkylthiophenes and alkylenedioxythiophenes
    7.
    发明授权
    Process for the preparation of dialkylthiophenes and alkylenedioxythiophenes 有权
    制备二烷基噻吩和亚烷基二氧噻吩的方法

    公开(公告)号:US06369239B2

    公开(公告)日:2002-04-09

    申请号:US09813875

    申请日:2001-03-21

    IPC分类号: C07D49504

    摘要: A process for the preparation of dialkoxythiophenes and alkylene-dioxythiophenes in high purity and very good yields by decarboxylation of dialkoxythiophene-dicarboxylic acids or alkylenedioxythiophenedicarboxylic acids, respectively, in solvents that have a higher boiling point than the product and contain no nitrogen bases.

    摘要翻译: 在沸点高于不含氮基的溶剂中分别通过二烷氧基噻吩 - 二羧酸或亚烷基二氧噻吩二羧酸脱羧来制备高纯度的二烷氧基噻吩和亚烷基二氧噻吩的方法。

    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.