HRID1740130

反应详情

EQUATION

反应方程式

HRID 1740130 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-hydroxy-1-(4-chloro-phenyl)-ethanone (4.7914 g, 28 mmol), prepared in the previous step, isopropyl isocyanate (4.1 ml, 42 mmol) and triethylamine (2.83 ml, 28 mmol) in 100 ml of benzene was refluxed under nitrogen for approximately 24 hours. The solid formed was collected by filtration and dried under high vacuum to give 3.5184 g (49%) of isopropyl-carbamic acid 2-(4-chloro-phenyl)-2-oxo-ethyl ester as an off-white solid. Recrystallization of a portion of this solid from isopropyl alcohol gave an analytically pure sample, mp 163-164° C.

WORKUP

后处理

  1. temperaturewas refluxed under nitrogen for approximately 24 hours
  2. customThe solid formed
  3. filtrationwas collected by filtration
  4. customdried under high vacuum