反应详情

To a suspension of methyl valinate hydrochloride (10.0 g, 59.7 mmol) and sodium carbonate (15.8 g, 149 mmol) in acetone (200 ml)-water (100 mL) was added 4-bromobenzenesulfonyl chloride (12.7 g, 49.7 mmol) at 0° C., and the mixture was stirred at room temperature for 12 hr after addition. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with ethyl acetate, washed with 0.1N hydrochloric acid, water and saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was crystallized from hexane-ethyl acetate to give the title compound as a white powder (14.7 g, 84%).

1. additionafter addition
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. additionthe residue was diluted with ethyl acetate
4. washwashed with 0.1N hydrochloric acid, water and saturated brine
5. dry with materialdried over sodium sulfate
6. customThe solvent was evaporated under reduced pressure
7. customthe residue was crystallized from hexane-ethyl acetate