HRID1762298

反应详情

EQUATION

反应方程式

HRID 1762298 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

In this example 36.1 g of 3-trifluoromethylbenzylsulfonyl chloride was added cautiously to a solution containing 29.8 g of the hydrochloride salt of methylaminoacetonitrile and 38.7 g of potassium carbonate in 130 ml of water at room temperature. The reaction mixture was maintained at about 70° C. for about four hours. The mixture was allowed to cool and then extracted with ethyl ether. The ethyl ether extract was dried over magnesium sulfate and evaporated to dryness. The residue was vacuum filtered through silica gel using 3% vol. tetrahydrofuran: chloroform as eluent. 29 g of the title compound was obtained as a waxy white solid.

WORKUP

后处理

  1. temperatureto cool
  2. extractionextracted with ethyl ether
  3. extractionThe ethyl ether extract
  4. dry with materialwas dried over magnesium sulfate
  5. customevaporated to dryness
  6. filtrationfiltered through silica gel using 3% vol. tetrahydrofuran