HRID1436011

反应详情

EQUATION

反应方程式

HRID 1436011 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

m-Chloroperbenzoic acid (1.4 g, 75%) was added in portions to a stirred solution of 5-bromo-6-methoxyisoquinoline (12 g, 5.04 mmol) in dichloromethane (12 ml). The mixture was stirred for 1 h then further dichloromethane (10 ml) added and the mixture stirred for an additional 2 h. Methanol (12 ml) was added and the mixture concentrated in vacuo to ˜9 ml, then 1M hydrochloric acid in diethyl ether (10 ml) was added. The mixture was diluted with ether and filtered, the precipitated solid was washed with diethyl ether and dried in vacuo to give crude 5-bromo-6-methoxyisoquinoline-N-oxide hydrochloride (1.22 g).

WORKUP

后处理

  1. stirringthe mixture stirred for an additional 2 h
  2. concentrationthe mixture concentrated in vacuo to ˜9 ml
  3. addition1M hydrochloric acid in diethyl ether (10 ml) was added
  4. additionThe mixture was diluted with ether
  5. filtrationfiltered
  6. washthe precipitated solid was washed with diethyl ether
  7. customdried in vacuo