反应详情

To a stirred solution of Intermediate 35, 4 isomers, one being (1S,2S)-1-Hydroxymethyl-2-phenyl-3-aza-bicyclo[3.1.0]hexane-3-carboxylic acid [(R)-1-(3,5-bis-trifluoromethyl-phenyl)-ethyl]-methyl-amide (0.28 g, 0.57 mmol) and triethylamine (0.13 mL, 0.96 mmol) in methylene chloride (6 mL) at 0° C. was added methanesulfonyl chloride (0.06 mL, 0.79 mmol). The reaction was allowed to warm to room temperature and stir for 2 hours. The reaction was washed with cold 0.5N HCl and the phases separated. The methylene chloride was washed with cold 0.5N NaOH, washed with brine, and dried over sodium sulfate, filtered and concentrated to give the title compound as a pink foam (0.32 g, quantitative yield). This material was processed without further purification.

1. washThe reaction was washed with cold 0.5N HCl
2. customthe phases separated
3. washThe methylene chloride was washed with cold 0.5N NaOH
4. washwashed with brine
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated