HRID2304295

反应详情

EQUATION

反应方程式

HRID 2304295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

At room temperature 58 g of m-chloroperoxybenzoic acid (purity 75%) were added in portions to a stirred solution of 7-methoxy-isoquinoline (35.9 g) in 500 mL of dichloromethane. Stirring was continued for 3 hours and subsequently methanol (400 mL) was added. The bulk was reduced to 300 mL and 325 mL of a saturated solution of hydrogen chloride in diethyl ether were added. Dilution with 600 mL of diethyl ether afforded precipitation of yellow crystals, which were separated by filtration, washed with chilled diethyl ether and dried in vacuo. Yield: 41.3 g (87%); m.p. 185-187° C.; (+)-FAB-MS: 176 (MH+-HCl).

WORKUP

后处理

  1. additionwere added
  2. customprecipitation of yellow crystals, which
  3. customwere separated by filtration
  4. washwashed with chilled diethyl ether
  5. customdried in vacuo