反应详情

10.5 g (0.25 mole) of cyanamide are dissolved in 250 ml of 2N potassium hydroxide solution and the solution so obtained is cooled to +10° C. At this temperature 26.5 ml (0.25 mole) of 2-bromopropionyl bromide are added dropwise and the reaction mixture is stirred for one hour at the same temperature. Then 16.8 g (0.2 mole) of sodium bicarbonate are added. 63 g (0.5 mole) of dimethylsulfate are subsequnetly added dropwise at 20° C. and the reaction mixture is stirred for 4 hours and extracted with methylene chloride. The combined organic phases are dried over sodium sulfate and concentrated by evaporation, affording as residue 27.5 g of crude product. Vacuum distillation of this crude products yields 13.6 g (28.5% of theory) of 2-bromopropionic acid N-cyano-N-methylamide with a boiling point of 45°-47° C. at 0.008 mbar.

1. customthe solution so obtained
2. temperatureis cooled to +10° C
3. stirringthe reaction mixture is stirred for 4 hours
4. extractionextracted with methylene chloride
5. dry with materialThe combined organic phases are dried over sodium sulfate
6. concentrationconcentrated by evaporation
7. customaffording as residue 27.5 g of crude product
8. distillationVacuum distillation of this crude products