HRID1070555

反应详情

EQUATION

反应方程式

HRID 1070555 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

At room temperature 133 g of m-chloroperbenzoic acid (purity 75%) was added in portions to a stirred solution of 6-methoxy-isoquinoline [Hendrickson, J. B.; 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. Yield: 85 g (80%); white solid; m.p. 189-191° C.; (+)-FAB-MS: 176 (MH+-HCl).

WORKUP

后处理

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