HRID973660

反应详情

EQUATION

反应方程式

HRID 973660 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 are added to a solution of 6.6 g (16.4 mmol) of the compound from Example II in 200 ml of methylene chloride p.A. and the mixture is stirred at room temperature for 1 hour. It is then filtered through kieselguhr with suction, and the methylene chloride phase is extracted 3 times with 100 ml of water each time and dried over magnesium sulphate. After concentrating in vacuo, the residue is chromatographed on a column (100 g of silica gel 70-230 mesh, φ 3.5 cm, using ethyl acetate/ petroleum ether 1:9)

WORKUP

后处理

  1. filtrationIt is then filtered through kieselguhr with suction
  2. extractionthe methylene chloride phase is extracted 3 times with 100 ml of water each time
  3. dry with materialdried over magnesium sulphate
  4. concentrationAfter concentrating in vacuo
  5. customthe residue is chromatographed on a column (100 g of silica gel 70-230 mesh, φ 3.5 cm, using ethyl acetate/ petroleum ether 1:9)