反应详情

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 an 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 were collected, giving 0.75 g of 4-(6-fluoro-3,4-dihydroxyphenyl)-7,8-dihydroxy-1,2,3,4-tetrahydroisoquinoline hydrobromide.

1. temperatureat an 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 dropwise
4. stirringThe mixture was stirred for 30 minutes at room temperature
5. customthe crystals which separated out
6. customwere collected