HRID54678

反应详情

EQUATION

反应方程式

HRID 54678 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.90 g of 4-(6-fluoro-3,4-dimethoxyphenyl)-7,8-dimethoxy-1,2,3,4-tetrahydroisoquinoline was dissolved in 25 ml of dichloromethane; and to the mixture was added dropwise 1M boron tribromide-dichloromethane solution (27 ml) under an argon gas stream, at internal temperature of -30° to -60° C. under cooling while stirring. The mixture was stirred for 3 hours at room temperature and 7.0 ml of methanol was added to the mixture under cooling with dry ice-methanol bath, dropwise. The mixture was stirred for 30 minutes at room temperature, the crystals which separated out was collected, giving 0.75 g of 4-(6-fluoro-3,4-dihydroxyphenyl)-7,8-dimethoxy-1,2,3,4-tetrahydroisoquinoline hydrobromide.

WORKUP

后处理

  1. temperatureat internal temperature of -30° to -60° C. under cooling
  2. stirringThe mixture was stirred for 3 hours at room temperature
  3. temperatureunder cooling with dry ice-methanol bath
  4. stirringThe mixture was stirred for 30 minutes at room temperature
  5. customthe crystals which separated out
  6. customwas collected