反应详情

α-[[(2,3-dimethoxybenzyl)amino]methyl]-6-fluoro-3,4-dimethoxybenzyl alcohol (1.0 g) was dissolved in 7 ml of trifluoroacetic acid, and after adding thereto under ice cooling, conc. sulfuric acid (0.25 ml), the mixture was stirred for 40 minutes. 0.72 g of sodium acetate was added to the reaction mixture, and the 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. After separating procedure, the chloroform layter was collected, washed with saturated aqueous NaCl solution, and dried over anhydrous sodium sulfate. The solvent was distilled off, 0.94 g of 4-(6-fluoro-3,4-dimethoxyphenyl)-7,8-dimethoxy-1,2,3,4-tetrahydroisoquinoline was obtained as a syrupy matter.

1. additionafter adding
2. concentrationthe 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 cooling
5. customAfter separating procedure
6. customthe chloroform layter was collected
7. washwashed with saturated aqueous NaCl solution
8. dry with materialdried over anhydrous sodium sulfate
9. distillationThe solvent was distilled off