HRID67087

反应详情

EQUATION

反应方程式

HRID 67087 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 81.5 g of 3,4-dichlorophenol, 98.0 g of anhydrous K2CO3, 40.0 g of chloroacetonitrile and 100 ml of DMSO was stirred and heated to 70° C. after an initial period of ice cooling. The reaction mixture was heated at 70°-80° C. for 3 hours and the reaction mixture was then poured into 2500 ml of ice and water which resulted in crystal formation. The crystals were removed by filtration, washed with water and then dried overnight in a vacuum oven. The resulting solids were put in approximately 1 liter of boiling cyclohexane and treated with activated charcoal and then filtered. The filtrate was cooled to 10° C. and filtered, which gave 91.5 g of 3,4-dichlorophenoxyacetonitrile, m.p. 61°-62° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated at 70°-80° C. for 3 hours
  2. customresulted in crystal formation
  3. customThe crystals were removed by filtration
  4. washwashed with water
  5. customdried overnight in a vacuum oven
  6. additiontreated with activated charcoal
  7. filtrationfiltered
  8. temperatureThe filtrate was cooled to 10° C.
  9. filtrationfiltered