HRID2116863
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationthe precipitate of NaCl is filtered off
- distillationThe solvent of the filtrate is subsequently distilled off
- customthe residue obtained
- customis dried for 1 hour at an oil-bath temperature of 50° C. under reduced pressure at 7.0 Pa