HRID54682

反应详情

EQUATION

反应方程式

HRID 54682 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.15 g of 4-(6-fluoro-3,4-dimethoxyphenyl)-1,2,3,4-tetrahydroisoquinoline was dissolved in 30 ml of dichloromethane, 26.4 ml of 1M boron tribromide-dichloromethane solution was added to the solution under an argon gas stream under stirring under cooling at the internal temperature of -20° to -30° C. The mixture was stirred for 3 hours at room temperature, and then, 7.0 ml of methanol was added dropwise under cooling in dry ice-methanol bath. The mixture was stirred for 30 minutes at room temperature, the crystals which separated out were collected by filtration, affording 1.0 g of 4-(6-fluoro-3,4-dihydroxyphenyl)-1,2,3,4-tetrahydroisoquinoline hydrobromide.

WORKUP

后处理

  1. temperatureunder cooling at the internal temperature of -20° to -30° C
  2. stirringThe mixture was stirred for 3 hours at room temperature
  3. stirringThe mixture was stirred for 30 minutes at room temperature
  4. customthe crystals which separated out
  5. filtrationwere collected by filtration