HRID1278072

反应详情

EQUATION

反应方程式

HRID 1278072 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add (dropwise, at room temperature, with stirring) 50.0 g of 2-dimethylamino-1-methyl-1-pyrrolinium-methylsulfate to 12.65 g of sodium methylate, suspended in 120 ml of absolute diethyl ether and boil the resulting reaction mixture under reflux for 1 hour. After cooling the refluxed material, filter the precipitated salt therefrom. Draw off the ether from the filtrate and distil under a vacuum what remains of the filtrate to obtain 9.0 g of the title compound as a liquid (with a very marked tendency to decomposition) of b.p. 45° to 47° at 11 mm of Hg.

WORKUP

后处理

  1. additionAdd (dropwise, at room temperature
  2. customthe resulting reaction mixture
  3. temperatureunder reflux for 1 hour
  4. temperatureAfter cooling the refluxed material
  5. filtrationfilter the precipitated salt
  6. customDraw off the ether from the filtrate and distil under a vacuum what