HRID17518

反应详情

EQUATION

反应方程式

HRID 17518 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

4-Fluoro-2-hydroxybenzoic acid (29.01 g, 0.186 mol) was dissolved in acetic acid (290 ml), then a solution of bromine (31.18 g, 0.195 mol) dissolved in acetic acid (15 ml) was gradually dropwise added at room temperature (1 hour). After stirred at 60° C. for 24 hours, this was cooled to room temperature. The reaction liquid was dried to solidness under reduced pressure, the residue was dissolved in methanol (100 ml), and this was poured into water (600 ml). After stirring at room temperature for 15 minutes, the precipitated crystal was washed and collected by filtration, and dried to obtain the entitled compound (35.36 g, 93%) as a colorless solid.

WORKUP

后处理

  1. additionwas gradually dropwise added at room temperature (1 hour)
  2. temperaturethis was cooled to room temperature
  3. customThe reaction liquid
  4. customwas dried to solidness under reduced pressure
  5. dissolutionthe residue was dissolved in methanol (100 ml)
  6. additionthis was poured into water (600 ml)
  7. stirringAfter stirring at room temperature for 15 minutes
  8. washthe precipitated crystal was washed
  9. filtrationcollected by filtration
  10. customdried