反应详情

985 g of dimethyl sulfate were added to 790 g (7.8 moles) of N,N-diethylformamide while stirring, in the course of which the internal temperature rose to 40°C. After the batch had been stirred overnight, the mixture was allowed to run into 7.8 moles of sodium methylate in methanol (total volume approximately 2.3 l) at 0° to 5°C, while stirring, and the reaction mixture was again stirred overnight. The methanol was then distilled from the crystal paste. The desired product was subsequently distilled off up to a bath temperature of 170°C under 10 mm Hg, and was then fractionally distilled through a column. 862 g (75% of theory) of N,N-diethylformamide-dimethylacetal of boiling point 70°C/50 mm Hg (foaming) and of refractive index nD24 of 1.4074 were obtained.

1. customrose to 40°C
2. stirringAfter the batch had been stirred overnight
3. stirringwhile stirring
4. distillationThe methanol was then distilled from the crystal paste
5. distillationThe desired product was subsequently distilled off up to a bath temperature of 170°C under 10 mm Hg
6. distillationwas then fractionally distilled through a column
7. customof 1.4074 were obtained