HRID1492164

反应详情

EQUATION

反应方程式

HRID 1492164 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

56.7 g. ( 0.42 mole ) 3-acetamidoaniline in 400 ml. dichloromethane and 65 ml. ( 0.46 tool ) triethylamine are mixed, while cooling with ice, with 59.0 g. (0.46 mole) 3,3-dimethylacryloyl chloride and stirred for 2 hours at ambient temperature. The solution is thereafter extracted with water and the separated organic phase is dried over anhydrous sodium sulphate, evaporated and the residue mixed with ethyl acetate. Upon standing in a refrigerator, crystals separate out. Yield 45.7 g. (47% of theory); m.p. 144°-148° C.

WORKUP

后处理

  1. temperaturewhile cooling with ice, with 59.0 g
  2. extractionThe solution is thereafter extracted with water
  3. dry with materialthe separated organic phase is dried over anhydrous sodium sulphate
  4. customevaporated
  5. additionthe residue mixed with ethyl acetate
  6. customseparate out