反应详情

α-[(benzylamino)methyl]-6-fluoro-3,4-dimethoxybenzyl alcohol (1.25 g) was dissolved in 8.75 ml of trifluoroacetic acid, and after adding thereto 0.37 ml of conc. sulfuric acid under ice-cooling, the mixture was stirred for 70 minutes. Then, 1.07 g of sodium acetate was added to the mixture, and the reaction mixture was concentrated. To the residue, was added chloroform and water, and the mixture was basified by addition of conc. aqueous ammonia under ice-cooling. By a separating procedure, the chloroform layer was collected, washed with saturated aquous NaCl solution, and dried over anhydrous sodium sulfate. The solvent was removed by distillation, giving 1.18 g of 4-(6-fluoro-3,4-dimethoxyphenyl)-1,2,3,4-tetrahydroisoquinoline as a syrupy matter.

1. additionafter adding
2. concentrationthe reaction mixture was concentrated
3. additionTo the residue, was added chloroform and water
4. additionthe mixture was basified by addition of conc. aqueous ammonia under ice-
5. temperaturecooling
6. customBy a separating procedure, the chloroform layer was collected
7. washwashed with saturated aquous NaCl solution
8. dry with materialdried over anhydrous sodium sulfate
9. customThe solvent was removed by distillation