反应详情

Aminoacetonitrile sulfate (H2NCH2CN.1/2H2SO4, 121.5 g, 1.156mole) was dissolved in water (230.9 g) and the solution was cooled to 0° to 5° C. and adjusted to pH 5 to 7 by the addition of a small amount of 30% aqueous sodium hydroxide solution. Ethyl chloroformate (108.5 g, 1.00 mole) and 30% aqueous sodium hydroxide solution were concurrently added dropwise with stirring and keeping pH at 5 to 7 at 0° to 5° C. over 2 hours and the mixture was stirred at the same temperature for additional 2 hours while keeping the same pH by dropping, if necessary, 30% aqueous sodium hydroxide solution. The total amount of 30% aqueous sodium hydroxide solution was 294.3 g. The reaction mixture was extracted three times with toluene (485 ml). The toluene layer was dried over anhydrous magnesium sulfate, toluene was evaporated and the residue was cooled to room temperature to give crystals (124.7 g, 0.968 mole) of ethyl N-cyanomethylcarbamate.

1. temperaturethe solution was cooled to 0° to 5° C.
2. customat 0° to 5° C.
3. customover 2 hours
4. stirringthe mixture was stirred at the same temperature for additional 2 hours
5. extractionThe reaction mixture was extracted three times with toluene (485 ml)
6. dry with materialThe toluene layer was dried over anhydrous magnesium sulfate, toluene
7. customwas evaporated