HRID1389571

反应详情

EQUATION

反应方程式

HRID 1389571 的结构方程式

PROCEDURE

实验过程

A suspension of 45.3 g. of 1-benzyloxy-2-[(2,6-dichlorophenyl)imino]-imidazolidine in 450 ml. of 48% strength hydrobromic acid is warmed to 80° for 4 hours. The resulting solution is poured onto ice and extracted with ether. The aqueous phase is evaporated in vacuo. The residue is distilled azeotropically five times with a mixture of ethanol/ethyl acetate. 2-[(2,6-dichlorophenyl)imino]-1-hydroxyimidazolidine hydrobromide is obtained by crystallization from a mixture of ethanol/ethyl acetate/ether. An analytically pure sample, m.p. 233°-234°, is obtained by recrystallization from methanol/acetonitrile.

WORKUP

后处理

  1. additionA suspension of 45.3 g
  2. additionThe resulting solution is poured onto ice
  3. extractionextracted with ether
  4. customThe aqueous phase is evaporated in vacuo
  5. distillationThe residue is distilled azeotropically five times
  6. additionwith a mixture of ethanol/ethyl acetate