HRID2116862
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
10.5 g (143.6 mmol) of diethylamine are added with stirring and cooling to 12.0 g (47.9 mmol) of bis(dimethylamino)chlorocarbenium tetracyanoborate. The reaction mixture is stirred for 3 hours at room temperature, and 30 ml of water are then added. The lower phase is separated off and diluted with 30 ml of dichloromethane. The organic phases are subsequently washed a number of times with 30 ml of water and dried using MgSO4. The solvent is then distilled off, and the residue is dried for 3 hours under reduced pressure at 7 Pa and 60° C., giving 13.4 g of N,N,N′,N′-tetramethyl-N″,N″-diethylguanidinium tetracyanoborate as a liquid, corresponding to a yield of 97.4%.
WORKUP
后处理
- stirringThe reaction mixture is stirred for 3 hours at room temperature
- customThe lower phase is separated off
- additiondiluted with 30 ml of dichloromethane
- washThe organic phases are subsequently washed a number of times with 30 ml of water
- customdried
- distillationThe solvent is then distilled off
- customthe residue is dried for 3 hours under reduced pressure at 7 Pa and 60° C.