HRID458440

反应详情

EQUATION

反应方程式

HRID 458440 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of tert-butyl (2S)-2-(3-ethoxy-3-oxopropanoyl)-1-pyrrolidinecarboxylate (5.0 g, 17.5 mmol) in benzene (50 ml) and piperidine (0.3 ml, 3 mmol) was added 4-carboxybenzaldehyde (2.63 g, 17.5 mmol), and the mixture was refluxed for 3 h. The cooled solution was washed with 0.1 N HCl twice. The aqueous layer was extracted three times with ether. The combined organic phases were dried (Na2SO4) and concentrated to give C as a tan solid (5.54 g, 76% yield). LCMS m/z 416 (M−H), 833 (2M−H).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 3 h
  2. washThe cooled solution was washed with 0.1 N HCl twice
  3. extractionThe aqueous layer was extracted three times with ether
  4. dry with materialThe combined organic phases were dried (Na2SO4)
  5. concentrationconcentrated