HRID46721

反应详情

EQUATION

反应方程式

HRID 46721 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution containing 54.0 g (0.385 mol) of 1-methylcyclopropanecarboxylic acid hydrazide (m.p. 72°-74°) and 90 g (0.9 mol) of phosgene in 1000 ml of ethyl acetate was refluxed for 2 hours. The reaction mixture was concentrated on a rotary evaporator. The residual solid crystallized from ether-hexane (1:5) to give 56.0 g (85%) of product as a white crystalline solid; m.p. 77°-78°.

WORKUP

后处理

  1. temperaturewas refluxed for 2 hours
  2. concentrationThe reaction mixture was concentrated on a rotary evaporator
  3. customThe residual solid crystallized from ether-hexane (1:5)