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Drugs intermediates 2,5-dichlorobenzoic acid synthesis method

机译:药物中间体2,5-二氯苯甲酸的合成方法

摘要

Drugs intermediates 2,5-dichlorobenzoic acid synthesis method, comprises the following steps: 2 mol 2,5-dichloro-6-aminobenzoic acid, 3-5 mol diisobutyl adipate solution were added to the reaction vessel, the temperature of the solution was raised to 70-78 and the stirring speed was controlled at 130-160 rpm, 3-4 mol cobalt naphthenate was added by 3-5 times, each time the interval was about 30-40 min, continued to react for 90-120 min, added 1200 ml potassium chloride solution, after the solution layered, reduced the solution temperature to 10-15 °C, added oxalic acid solution to adjust the pH to 4-5, washed with potassium sulfate solution, washed with methyl tert-butyl ether solution, and washed with 2-methyl tetrahydrofuran solution, vacuum distillation, collected fractions of 110-120 °C, dehydrated with dehydrating agent, finally obtained 2,5-dichlorobenzoic acid.
机译:药物中间体2,5-二氯苯甲酸的合成方法,包括以下步骤:将2mol的2,5-二氯-6-氨基苯甲酸,3-5mol的己二酸二异丁酯溶液加入反应容器中,升高溶液温度达到70-78,并将搅拌速度控制在130-160 rpm,将3-4 mol环烷酸钴加入3-5次,每次间隔约30-40分钟,继续反应90-120分钟,加入1200 ml氯化钾溶液,溶液分层后,降低溶液温度至10-15°C,加入草酸溶液将pH值调节至4-5,用硫酸钾溶液洗涤,用甲基叔丁基醚溶液洗涤并用2-甲基四氢呋喃溶液洗涤,真空蒸馏,收集110-120℃的馏分,用脱水剂脱水,最后得到2,5-二氯苯甲酸。

著录项

  • 公开/公告号IES86994B2

    专利类型

  • 公开/公告日2019-05-01

    原文格式PDF

  • 申请/专利权人 CHENGDU DONG DIAN AI ER TECHNOLOGY CO.LTD;

    申请/专利号IES20180089

  • 发明设计人 YIDA YAN;

    申请日2018-04-03

  • 分类号C07C51;C07C63;

  • 国家 IE

  • 入库时间 2022-08-21 12:02:17

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