HRID515278

反应详情

EQUATION

反应方程式

HRID 515278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe reaction was concentrated under reduced pressure and water
  2. additionwas added
  3. additionSolid sodium hydrogen carbonate was added portionwise until no further gas
  4. extractionThe aqueous mixture was extracted with ethyl acetate
  5. dry with materialThe organic phase was dried (magnesium sulfate)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure