HRID1366737

反应详情

EQUATION

反应方程式

HRID 1366737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

At ambient temperature 133 g of m-chloroperbenzoic acid (purity 75%) was added in portions to a stirred solution of 6-methoxy-isoquinoline [Hendricks, J. B. and Rodriguez, C., J. Org. Chem. 1983, 48, 3344-3346; 79.8 g; 500 mmol] in 1.2 L of dichloromethane. Stirring was continued for 3 hours and subsequently methanol (1 L) was added. The bulk was reduced to 700 ml after which 800 ml of a saturated solution of hydrogen chloride in diethyl ether was added. Dilution with 1.5 L of diethyl ether resulted in precipitation of yellow crystals, which were separated by filtration, washed with chilled diethyl ether and dried in vacuo to give 6-methoxy-isoquinoline-N-oxide hydrochloride (85 g, 80%), (+)-FAB-MS 176 [M+H-HCl]+.

WORKUP

后处理

  1. additionwas added
  2. customwere separated by filtration
  3. washwashed with chilled diethyl ether
  4. customdried in vacuo