反应详情

温度

70 °C

To a solution of (2R,4R)-1-allyloxycarbonyl-4-(t-butyldimethylsilyloxy)-2-(2-methanesulfonyloxyethyl) pyrrolidine (37.6 g) and ammonium chloride (5.84 g) in dimethylformamide (185 ml) was added portionwise sodium azide (7.1 g) at ambient temperature. The mixture was stirred at 70° C. for 3 hours, and poured into a mixture of ethyl acetate and water. The organic layer was separated and the aqueous layer was extracted twice with ethyl acetate. The combined organic layer was washed twice with water and once with brine, dried over magnesium sulfate and evaporated under reduced pressure to give (2R,4R)-1-allyloxycarbonyl-2-(2-azidoethyl)-4-(t-butyl-dimethylsilyloxy) pyrrolidine (29.7 g).

1. customThe organic layer was separated
2. extractionthe aqueous layer was extracted twice with ethyl acetate
3. washThe combined organic layer was washed twice with water and once with brine
4. dry with materialdried over magnesium sulfate
5. customevaporated under reduced pressure