HRID1632729

反应详情

EQUATION

反应方程式

HRID 1632729 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 4.9 g (0.064 moles) propanthiol and 3 g (0.054 moles) potassium hydroxide in 50 ml dimethylsulfoxide was heated (at about 120° C.) for thirty minutes. Then 10 g (0.054 moles) 1-methyl-3,4,5-trichloropyrazole was added in one portion. Heating (at about 120° C.) of the stirred reaction mixture was continued for about 6 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, washed with water twice, and dried over magnesium sulfate. The solvent was then stripped. The product was distilled out at 124° C. under high vacuum and heat.

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. washwashed with water twice
  7. dry with materialdried over magnesium sulfate
  8. distillationThe product was distilled out at 124° C. under high vacuum
  9. temperatureheat