反应详情

温度

100 °C

To a solution of an optically-active compound of 3-(1,1-difluoro-allyl)-piperidine-1,3-dicarboxylic acid 1-tert-butyl ester (12.3 g) and triethylamine (11.2 ml) in toluene (123 ml) heated to 100° C. was added dropwise diphenylphosphoryl azide (11.2 ml). The reaction mixture was stirred at 100° C. for 25 minutes, and then thereto were added benzyl alcohol (6.2 ml) and 4-dimethylaminopyridine (0.98 g). The mixture was stirred at 100° C. overnight, and then cooled to room temperature and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=9/1 to 85/15) to give the titled compound (15.1 g).

1. stirringThe mixture was stirred at 100° C. overnight
2. temperaturecooled to room temperature
3. concentrationconcentrated under reduced pressure
4. customThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=9/1 to 85/15)