HRID580257

反应详情

EQUATION

反应方程式

HRID 580257 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

A mixture of 1-(2-fluoro-4-chloro-5-methylsulfonyloxyphenyl)- 3,4,5-trimethylpyrazole (33.3 g), 2N aqueous sodium hydroxide (100 ml) and ethanol (50 ml) was stirred at 40° C. for 30 minutes. After cooling, the reaction mixture was acidified with aqueous hydrochloric acid and then extracted wth toluene. The toluene layer thus obtained was washed with water and dried over anhydrous sodium sulfate. Removal of the solvent by distillation in vacuo gave the titled compound (24.2 g) as a pale yellow crystalline solid. Recrystallization of this solid from a mixture of n-hexane/ethyl acetate yielded a white crystalline solid. m.p. 158°-160° C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionextracted wth toluene
  3. customThe toluene layer thus obtained
  4. washwas washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customRemoval of the solvent
  7. distillationby distillation in vacuo