HRID217436

反应详情

EQUATION

反应方程式

HRID 217436 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

The suspension of 4-bromo-5-ethylthiophene-2-carboxylic acid (800 mg) in MeOH (4 mL) was added dropwise SOCl2 (0.50 mL) at 0° C. The reaction mixture was stirred at 0° C. for 1 hour, warmed to 60° C., and then stirred for 15 hours. The reaction liquid was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (automatic purification device, hexane:EtOAc=98:2 to 70:30) to obtain methyl 4-bromo-5-ethylthiophene-2-carboxylate (765.0 mg) as a colorless liquid.

WORKUP

后处理

  1. temperaturewarmed to 60° C.
  2. stirringstirred for 15 hours
  3. customThe reaction liquid
  4. concentrationwas concentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (automatic purification device, hexane:EtOAc=98:2 to 70:30)