HRID2116862

反应详情

EQUATION

反应方程式

HRID 2116862 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringThe reaction mixture is stirred for 3 hours at room temperature
  2. customThe lower phase is separated off
  3. additiondiluted with 30 ml of dichloromethane
  4. washThe organic phases are subsequently washed a number of times with 30 ml of water
  5. customdried
  6. distillationThe solvent is then distilled off
  7. customthe residue is dried for 3 hours under reduced pressure at 7 Pa and 60° C.