HRID651248

反应详情

EQUATION

反应方程式

HRID 651248 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of ethyl 2-azidoacetate (1.29 g) and 2-chloroacrylonitrile (1.75 g) in water (10 ml) is stirred at about 80° C. for 16 hours. After cooling, the product is extracted with dichloromethane and the concentrated extract is purified by means of column chromatography on silica gel 60 (6 g; eluent toluenelethyl acetate=4:1). The purified product (yield 1.21 g; 67% of theory) of m.p. 47-48° C. (recrystallization from toluene/hexane) is obtained after concentrating the eluate and drying.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionthe product is extracted with dichloromethane
  3. extractionthe concentrated extract
  4. customis purified by means of column chromatography on silica gel 60 (6 g; eluent toluenelethyl acetate=4:1)
  5. customThe purified product (yield 1.21 g; 67% of theory) of m.p. 47-48° C. (recrystallization from toluene/hexane)
  6. customis obtained
  7. concentrationafter concentrating the eluate and
  8. customdrying