HRID440502

反应详情

EQUATION

反应方程式

HRID 440502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-[2-(4-benzyloxy-3-methoxyphenyl)ethyl]-1-(2-methoxyphenyl)cyclopropane carboxamide (30.3 g) in acetonitrile (450 ml) and phosphoryl chloride (50 ml) was heated under reflux for 80 minutes. The solvent was evaporated in vacuo below 50° C. and the residue washed with ethyl acetate and then stirred with ethyl acetate (300 ml) and ice-cold 5% aqueous ammonia solution (200 ml) for 10 minutes. The organic layer was dried over potassium carbonate and the solvent removed by evaporation to give 7-benzyloxy-6-methoxy-1-[1-(2-methoxyphenyl)cyclopropyl]-3,4-dihydroisoquinoline.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 80 minutes
  3. customThe solvent was evaporated in vacuo below 50° C.
  4. washthe residue washed with ethyl acetate
  5. dry with materialThe organic layer was dried over potassium carbonate
  6. customthe solvent removed by evaporation