HRID1632730

反应详情

EQUATION

反应方程式

HRID 1632730 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A stirred mixture of 10.3 g (0.065 moles) 4-chlorobenzyl mercaptan and 3.0 g (0.054 moles) potassium hydroxide in 50 ml dimethylsulfoxide was heated (at about 120° C.) for about 20 minutes. Then 10 g (0.054 moles) 1-methyl-3,4,5-trichloropyrazole were added. Heating (at about 120° C.) of the stirred reaction mixture was continued for about 4 hours. The reaction mixture was allowed to cool. The reaction mixture was added to water (about 50 ml); the resulting mixture was extracted with ether. The etheral phase was separated and dried over magnesium sulfate. The solvent was stripped and the residue was hard-topped. The product was purified by high pressure liquid chromatography to give 6 g.

WORKUP

后处理

  1. temperatureHeating
  2. custom(at about 120° C.) of the stirred reaction mixture
  3. temperatureto cool
  4. extractionthe resulting mixture was extracted with ether
  5. customThe etheral phase was separated
  6. dry with materialdried over magnesium sulfate
  7. customThe product was purified by high pressure liquid chromatography
  8. customto give 6 g