反应详情

Stir a mixture of sodium hydride (115 mg, 2.89 mmol, 60% in mineral oil) in N-methyl-2-pyrrolidinone (960 μL) and 1-propanol (234 μL) for 10 minutes and then add a solution of (2R,3S,5R)-5-[(1S,2S)-1-benzyloxy-2-dibenzylamino-3-(3,5-difluorophenyl)-propyl]-2-(3-fluoro-2,2-dimethylpropoxy)-3-methylmorpholine-4-carboxylic acid tert-butyl ester (440 mg, 0.57 mmol) in N-methyl-2-pyrrolidinone (1 mL) and stir in a sealed vial at 90° C. for 4 hours. Cool to room temperature and pour reaction mixture into water and extract well with ethyl acetate. Wash the organic phase with water followed by saturated aqueous sodium chloride and concentrate under reduced pressure. Subject the resulting residue to silica gel chromatography, eluting with hexane containing from 0-50% ethyl acetate to provide the desired compound.

1. stirringstir in a sealed vial at 90° C. for 4 hours
2. additionpour
3. extractionextract well with ethyl acetate
4. washWash the organic phase with water
5. concentrationconcentrate under reduced pressure
6. washeluting with hexane containing from 0-50% ethyl acetate