反应详情

To a stirred solution of methyl 3-amino-5-bromo-2-methylbenzoate (1.0 g, 4.09 mmol) and acetaldehyde (180 mg, 4.09 mmol) in dichloroethane (10 mL), acetic acid (1.47 g, 24.58 mmol) was added and reaction stirred at room temperature for 30 minutes. Then sodium triacetoxyborohydride (2.6 g, 12.29 mmol) was added at 0° C., allowed to attain room temperature and stirring continued for 2 h. On completion, reaction mixture was diluted with dichloromethane, washed with water, saturated aqueous sodium bicarbonate solution and dried over sodium sulphate. Removal of the solvent under reduced pressure followed by column chromatographic purification afforded the desired compound (600 mg, 55%).

1. customreaction
2. customto attain room temperature
3. stirringstirring
4. waitcontinued for 2 h
5. customOn completion, reaction mixture
6. washwashed with water, saturated aqueous sodium bicarbonate solution
7. dry with materialdried over sodium sulphate
8. customRemoval of the solvent under reduced pressure
9. customfollowed by column chromatographic purification