HRID1278070

反应详情

EQUATION

反应方程式

HRID 1278070 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add (dropwise at 80°, with stirring) a solution of 3.5 g of sodium in 80 ml of ethanol to a mixture of 16.1 g of 3,4-methylenedioxybenzylcyanide and 36 g of 2-dimethylamino-1-methyl-1-pyrrolinium-methylsulfate. Continue boiling the resulting reaction mixture for a further 2 hours. Then distil off the solvent under a vacuum and take up the residue with water/diethyl ether. Collect the ethereal layer. Dry it over sodium sulfate and concentrate it to obtain 18 g (67% of theory) of the title compound as oily liquid.

WORKUP

后处理

  1. additionAdd (dropwise at 80°
  2. customthe resulting reaction mixture for a further 2 hours
  3. customThen distil off the solvent under a vacuum
  4. customCollect the ethereal layer
  5. dry with materialDry it over sodium sulfate
  6. concentrationconcentrate it