HRID324793

反应详情

EQUATION

反应方程式

HRID 324793 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.8 g (16.4 mmol) of 2,3-dichloro-5,6-dicyano-p-benzoquinone is added to a solution of 6.6 g (16.4 mmol) of 1,4-dihydro-2,6-diisopropyl-4-(4-fluorophenyl)pyridine-3,5-dicarboxylic acid diethylester in 200 ml of analysis grade methylene chloride, and the mixture is then stirred for 1 h at room temperature. After this, it is drawn off by suction over diatomaceous earth, and the methylene chloride phase is extracted 3 times with 100 ml of water each time and dried on magnesium sulfate. After concentrating in a vacuum, the residue is chromatographed on a column (100 g of silica gel, 70-230 mesh, diameter 3.5 cm, with ethyl acetate/petroleum ether 1:9).

WORKUP

后处理

  1. extractionthe methylene chloride phase is extracted 3 times with 100 ml of water each time
  2. customdried on magnesium sulfate
  3. concentrationAfter concentrating in a vacuum
  4. customthe residue is chromatographed on a column (100 g of silica gel, 70-230 mesh, diameter 3.5 cm, with ethyl acetate/petroleum ether 1:9)