反应详情

0.65 g of 4-(6-fluoro-3,4-dimethoxyphenyl)-4,5,6,7-tetrahydrothieno[2,3-c]pyridine was dissolved in 14 ml of dichloromethane; and to the mixture was added 1M boron tribromide-dichloromethane solution (12 ml) dropwise under an argon gas stream, while cooling at -30°--60° C. (internal temperature) while stirring. The mixture was stirred for 2 hours at room temperature, and 20 ml of methanol was added dropwise thereto under ice cooling. The solvent was distilled off, and the residue obtained was crystallized by using a mixture of methanol and chloroform (1:8). The crystals were collected by filtration, and recrystallized from ethanol, giving 0.29 g of 4-(6-fluoro-3,4-dihydroxyphenyl)-4,5,6,7-tetrahydrothieno[2,3-c]pyridine hydrobromide

1. temperaturewhile cooling at -30°--60° C. (internal temperature)
2. stirringThe mixture was stirred for 2 hours at room temperature
3. distillationThe solvent was distilled off
4. customthe residue obtained
5. customwas crystallized
6. additiona mixture of methanol and chloroform (1:8)
7. filtrationThe crystals were collected by filtration
8. customrecrystallized from ethanol