反应详情

温度

70 °C

221 g (2.085 mols) of sodium acetylcyanamide are dissolved in 500 ml of dimethylformamide at 90° C., the mixture is allowed to cool to 70° C. and 285.6 g (2.085 mols) of n-butyl bromide are then added dropwise at 70° C. in the course of 11/2 hours. The mixture is allowed to after-react at 70° C. for 10 hours, and the NaBr which has precipitated is filtered off with suction and the entire distillable constituent is removed from the filtrate by vacuum distillation. Fractional distillation of this distillate over a packed column 60 cm high gives 216.4 g (74.1% of theory) of pure product of boiling point 105° C./34 mbar.

1. customto after-react at 70° C. for 10 hours
2. customthe NaBr which has precipitated
3. filtrationis filtered off with suction
4. customthe entire distillable constituent is removed from the filtrate by vacuum distillation
5. distillationFractional distillation of this distillate over a packed column 60 cm
6. customhigh gives 216.4 g (74.1% of theory) of pure product of boiling point 105° C./34 mbar