HRID483572

反应详情

EQUATION

反应方程式

HRID 483572 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 mixture of 50.0 g of p-fluoronitrobenzene, 85.93 g of 2-methylimidazole and 44.9 g of potassium carbonate in 860 ml of dimethylsulfoxide is heated at 120° C. for 24 hours. The mixture is poured into 2.5 liter of water and stored in a refrigerator for two days. The mixture is filtered and cake washed with copious volumes of water and vacuum dried. The cake is dissolved in 1500 ml of ethyl acetate, filtered through hydrous magnesium silicate and the filtrate reduced to about 500 ml, cooled and the resulting solid, filtered, and air dried to give 81.0 g of the desired product as brown Crystals, m.p. 135°-137° C.

WORKUP

后处理

  1. filtrationThe mixture is filtered
  2. washcake washed with copious volumes of water and vacuum
  3. customdried
  4. dissolutionThe cake is dissolved in 1500 ml of ethyl acetate
  5. filtrationfiltered through hydrous magnesium silicate
  6. temperaturecooled
  7. filtrationthe resulting solid, filtered
  8. customair dried