HRID515278
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
tert-Butyl 4-(4-nitrobenzylidene)piperidine-1-carboxylate (31.4 mmol, 10 g) was stirred in a mixture of dichloromethane/trifluoroacetic acid for 3 hours. The reaction was concentrated under reduced pressure and water was added. Solid sodium hydrogen carbonate was added portionwise until no further gas was evolved. The aqueous mixture was extracted with ethyl acetate. The organic phase was dried (magnesium sulfate), filtered and concentrated under reduced pressure to give the title compound (5.2 g). MS (ESI) m/z 219.1 [M+H]+
WORKUP
后处理
- concentrationThe reaction was concentrated under reduced pressure and water
- additionwas added
- additionSolid sodium hydrogen carbonate was added portionwise until no further gas
- extractionThe aqueous mixture was extracted with ethyl acetate
- dry with materialThe organic phase was dried (magnesium sulfate)
- filtrationfiltered
- concentrationconcentrated under reduced pressure