HRID726087

反应详情

EQUATION

反应方程式

HRID 726087 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

15.6 g (0.124 mol) of sodium sulfite are dissolved in 120 ml of water at 70° C. While maintaining the temperature, 23.8 g (0.1 mol) of 4-fluoro-3-chlorosulfonylbenzoic acid and 10N NaOH are added simultaneously and in portions such that the pH is kept between 9 and 10 (exothermic reaction). The mixture is stirred for a further 3 hours at 70° C., stirred for a further 15 minutes with active carbon and then filtered. The filtrate is adjusted to pH 0-1 using concentrated hydrochloric acid with external cooling and the crystalline 5-carboxy-2-fluorobenzenesulfinic acid is filtered off.

WORKUP

后处理

  1. additionare added simultaneously and in portions such that the pH
  2. customis kept between 9 and 10 (exothermic reaction)
  3. stirringstirred for a further 15 minutes with active carbon
  4. filtrationfiltered
  5. temperaturewith external cooling
  6. filtrationthe crystalline 5-carboxy-2-fluorobenzenesulfinic acid is filtered off