反应详情

温度

60 °C

A mixture of N.N-dimethylformamide (7.31 g) and dimethylsulfate (12.60 g) are heated to 60° C. for 4 h. Then dimethylamine in THF (100 ml, 2 M solution) and toluene (15 ml) are added and the resulting mixture is stirred at reflux for 1 h. The reaction mixture is cooled to room temperature and the phases are separated. The lower layer is washed three times with anhydrous tert-butyl methyl ether to give N,N,N′,N′-tetramethylformamidinium methylsulfate (18, R6=Me, R7=Me). 1H NMR (C6D6), 7.95 (1H), 3.70 (3H), 3.32 (6H), 3.29 (6H).

1. temperatureat reflux for 1 h
2. temperatureThe reaction mixture is cooled to room temperature
3. customthe phases are separated
4. washThe lower layer is washed three times with anhydrous tert-butyl methyl ether