HRID54678
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat internal temperature of -30° to -60° C. under cooling
- stirringThe mixture was stirred for 3 hours at room temperature
- temperatureunder cooling with dry ice-methanol bath
- stirringThe mixture was stirred for 30 minutes at room temperature
- customthe crystals which separated out
- customwas collected