HRID1691778

反应详情

EQUATION

反应方程式

HRID 1691778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

3-(1-Benzoyl-4-oxo-1,2,3,4-tetrahydro-pyridin-2-yl)-benzonitrile (350 mg) was dissolved in 50 ml methanol at 0° C. and 1.5 ml of 0.5 M sodium methoxide in methanol was added. The solution was stirred at 0° C. for 3 hours, and then 25 ml of pH 7 phosphate buffer was added. The mixture was concentrated under reduced pressure and partitioned between buffer and ethyl acetate. The organic layer was dried over sodium sulfate and the drying agent filtered off. Racemic 2-(3-cyanophenyl)-2,3-dihydro-pyridin-4-one was crystallized by addition of hexane to give 131 mg.

WORKUP

后处理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. custompartitioned between buffer and ethyl acetate
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationthe drying agent filtered off
  5. customRacemic 2-(3-cyanophenyl)-2,3-dihydro-pyridin-4-one was crystallized by addition of hexane
  6. customto give 131 mg