HRID1248105

反应详情

EQUATION

反应方程式

HRID 1248105 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

78.8 parts of methyl chloroformate and a mixture of 46.8 parts of potassium hydroxide in 215 parts of water are added via two inlets to a mixture of 113.8 parts of isovaleramidine hydrochloride in 530 parts of methylene chloride, at from 0° to 10° C., in the course of 25 minutes, while stirring. The mixture is stirred at 25° C. for 30 minutes, the phases are separated and the aqueous phase is extracted once with methylene chloride. The solvent is removed from the organic extract to give 123 parts (93.3% of theory) of N-methoxycarbonylisovaleramidine of melting point 82°-86° C.

WORKUP

后处理

  1. stirringThe mixture is stirred at 25° C. for 30 minutes
  2. customthe phases are separated
  3. extractionthe aqueous phase is extracted once with methylene chloride
  4. customThe solvent is removed from the
  5. extractionorganic extract