HRID2116863

反应详情

EQUATION

反应方程式

HRID 2116863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.54 g (11.48 mmol) of sodium methylsulfate and 10 ml of dry acetonitrile are added under an inert-gas atmosphere to 1.96 g (11.46 mmol) of bis(dimethylamino)dichloromethane. The reaction mixture is stirred for 5 hours at room temperature, and the precipitate of NaCl is filtered off. The solvent of the filtrate is subsequently distilled off, and the residue obtained is dried for 1 hour at an oil-bath temperature of 50° C. under reduced pressure at 7.0 Pa, giving 2.78 g of bis(dimethylamino)chlorocarbenium methylsulfate as a viscous liquid, corresponding to a yield of 98.3%.

WORKUP

后处理

  1. filtrationthe precipitate of NaCl is filtered off
  2. distillationThe solvent of the filtrate is subsequently distilled off
  3. customthe residue obtained
  4. customis dried for 1 hour at an oil-bath temperature of 50° C. under reduced pressure at 7.0 Pa