HRID2220310

反应详情

EQUATION

反应方程式

HRID 2220310 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

Methyl 3-chloro-4-fluoro-7-methoxy-1-benzothiophene-2-carboxylate (2.00 g, 7.29 mmol) was suspended in THF:H2O[10:1] and lithium hydroxide (260 mg) added, the resulting suspension was heated to 40° C. for 1 h. After cooling to room temperature the mixture was extracted with diethyl ether (50 mL) and the aqueous phase acidified to pH 2 and the solid collected by filtration and vacuum dried to give a white solid (1.09 g, 58%); δH (300 M , DMSO) 7.32-7.20 (1H, m, Ar), 7.15-7.05 (1H, dd, Ar), 3.98 (3H, s, OCH3).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature the mixture
  2. extractionwas extracted with diethyl ether (50 mL)
  3. filtrationthe solid collected by filtration and vacuum
  4. customdried