HRID1248103

反应详情

EQUATION

反应方程式

HRID 1248103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

165 parts of methyl chloroformate and 141.8 parts of sodium hydroxide in 590 parts of water are added via two inlets to 221 parts of 2-methylpropionamidine hydrochloride in 1,000 parts of diethyl ether, at from 25° to 30° C., in the course of 40 minutes, while stirring. The mixture is stirred at room temperature for one hour, and the organic phase is separated off. The aqueous phase is extracted again with 200 parts of diethyl ether, and the solvent is removed from the combined organic extracts to give 223 parts (86% of theory) of N-methoxycarbonyl-2-methylpropionamidine of melting point 127°-130° C.

WORKUP

后处理

  1. stirringThe mixture is stirred at room temperature for one hour
  2. customthe organic phase is separated off
  3. extractionThe aqueous phase is extracted again with 200 parts of diethyl ether
  4. customthe solvent is removed from the combined organic extracts