反应详情

To a solution of methyl N-((benzyloxy)carbonyl)-4,4-difluoro-L-norvalinate (1.59 g, 5.29 mmol) in ethanol (50 mL) was added lithium chloride (919 mg) and the mixture was stirred for 10 minutes. Sodium borohydride (820 mg) was added slowly, the mixture stirred for 2 hours. Then, another portion of sodium borohydride (100 mg) was added and stirring continued for 30 minutes. The mixture was diluted with water (20 mL) and neutralized slowly with 1N HCl followed by the addition of another aliquot of water. The mixture was extracted with ethyl acetate (2×), washed with brine, dried over magnesium sulfate, filtered and the solvent evaporated under vacuum to afford benzyl (1S)-3,3-difluoro-1-(hydroxymethyl)butylcarbamate.

1. stirringthe mixture stirred for 2 hours
2. stirringstirring
3. waitcontinued for 30 minutes
4. extractionThe mixture was extracted with ethyl acetate (2×)
5. washwashed with brine
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. customthe solvent evaporated under vacuum