HRID267990

反应详情

EQUATION

反应方程式

HRID 267990 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of ethyl aminooxyacetate hydrochloride (18.0 g.) in water (64 cc.) is added to a stirred boiling solution of 7H-indolizino[5,6,7-ij]isoquinolin-7-one (16.0 g.) in ethanol (320 cc.) and pyridine (9.1 g.). Boiling is maintained for 3 hours 30 minutes. After cooling, water (640 cc.) is added. The greenish yellow crystals thus obtained are filtered off and washed with 25% ethanol and then with water. After drying, crude 7-ethoxycarbonylmethoxyimino-7H-indolizino[5,6,7-ij isoquinoline (21.6 g.) is obtained and is recrystallised from a mixture of ethyl acetate (110 cc.) and cyclohexane (165 cc.). 7-Ethoxycarbonylmethoxyimino- 7H-indolizino[5,6,7-ij]isoquinoline (13.1 g.), melting at 134° C., is thus obtained.

WORKUP

后处理

  1. temperatureBoiling is maintained for 3 hours 30 minutes
  2. temperatureAfter cooling
  3. customThe greenish yellow crystals thus obtained
  4. filtrationare filtered off
  5. washwashed with 25% ethanol
  6. customAfter drying
  7. customcrude 7-ethoxycarbonylmethoxyimino-7H-indolizino[5,6,7-ij isoquinoline (21.6 g.) is obtained
  8. customis recrystallised from a mixture of ethyl acetate (110 cc.) and cyclohexane (165 cc.)