利索-全球专利检索

  1. 登录
  2. 注册
发明公开
CN108623465A 一种利凡诺药物中间体2-氯-4-硝基苯甲酸的合成方法 无效 - 撤回

一种利凡诺药物中间体2-氯-4-硝基苯甲酸的合成方法
摘要：
一种利凡诺药物中间体2-氯-4-硝基苯甲酸的合成方法，主要包括如下步骤：在反应容器中加入3mol的2-氯-4-硝基-6-羟基-异丙基苯，4-6mol的N-甲基吗啉溶液，升高溶液温度至40—46℃，控制搅拌速度170—190rpm,保持50—70min之后，加入6mol的钛酸四正丙酯，升高溶液温度至50—55℃，回流90—110min,降低溶液温度至10—15℃，析出固体，过滤，固体用烯丙胺溶液洗涤，用草酸溶液调节pH至3-4，降低温度至5—8℃，析出晶体，过滤，用水杨酸甲酯溶液洗涤，脱水剂脱水，得成品2-氯-4-硝基苯甲酸。
摘要（英）：

The invention relates to a synthetic method of a rivanol medicine intermediate of 2-chlorine-4-nitrobenzoic acid. The synthetic method mainly comprises the following steps that 3mol of 2-chloro-4-nitryl-6-hydroxy-isopropyl benzene and 4 to 6mol of N-methylmorpholine solution are added into a reaction container; the solution temperature is raised to 40 to 46 DEG C; the stirring speed is controlledto be 170 to 190rpm and the temperature is maintained for 50 to 70min, 6mol of tetra-n-propyl titanate is added; the solution temperature is raised to be 50 to 55 DEG C; backflow is performed for 90 to 110min; the solution temperature is reduced to be 10 to 15 DEG C; solids are separated out; filtering is performed; the solids are washed by an allyl amine solution; the pH is regulated to be 3 to 4by an oxalic acid solution; the temperature is reduced to be 5 to 8 DEG C; crystals are separated out; filtering is performed; a methyl salicylate solution is used for washing; a dehydrating agent isused for dehydration; a finished product of 2-chloro-4-nitrobenzoic acid is obtained.

0/0