反应详情

温度

55 °C

A mixture of 15.1 g (41 mmol) (3S,4R)-1-Benzyl-4-(4-chloro-3-fluoro-phenyl)-pyrrolidine-3-carboxylic acid and 11.6 g (90 mmol) DIPEA in 100 mL t-butanol was heated to 55° C. and 12.4 g (45 mmol) diphenylphosphoryl azide was added. The mixture was heated to 80° C. for 3 h and evaporated. The residue was subjected to column chromatography on silica eluting with a gradient formed from ethyl acetate and heptane to yield after evaporation of the product containing fractions 5.7 g (34%) of the title compound as off-white solid. MS m/e: 405.3 [M+H]+.

1. temperatureThe mixture was heated to 80° C. for 3 h
2. customevaporated
3. customformed from ethyl acetate and heptane
4. customto yield
5. customafter evaporation of the product
6. additioncontaining fractions 5.7 g (34%) of the title compound as off-white solid