反应详情

A flask containing racemic Intermediate 24, one enantiomer being (1S,2S)-1-(3,5-bis-trifluoromethyl-benzyloxymethyl)-2-phenyl-3-aza-bicyclo[3.1.0]hexane-3-carboxylic acid tert-butyl ester (0.25 g, 0.49 mmol) and methylene chloride (10 mL) was immersed in a 0° C. bath. Trifluoroacetic acid (0.75 mL, 9.7 mmol) was added, and the reaction was stirred for 3 hours at room temperature. 20% NaOH solution was added cautiously and then saturated sodium bicarbonate solution was added until the pH=8. The phases were separated; the organics were washed with brine, dried over sodium sulfate, filtered, and concentrated to give the title compound (0.20 g, quantitative yield).

1. customwas immersed in a 0° C.
2. customThe phases were separated
3. washthe organics were washed with brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated