HRID403264

反应详情

EQUATION

反应方程式

HRID 403264 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 1-difluoromethyl-1H-pyrazole-3-carboxylic acid methyl ester (535 mg, 3 mmole) and N-chloro-succinimide (1.22 g, 9.1 mmole) in DMF (5 ml) was heated at 50° C. overnight. The reaction mixture was cooled, partitioned between AcOEt and water, the organic layer was washed with water, dried, evaporated and the residue was purified by chromatography on silica gel using cyclohexane/AcOEt (3:1) to give the title compound (540 mg) as a white solid. MS: m/z=209.9 [M]+.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. custompartitioned between AcOEt and water
  3. washthe organic layer was washed with water
  4. customdried
  5. customevaporated
  6. customthe residue was purified by chromatography on silica gel