反应详情

温度

95 °C

Cyanoacetic acid (28 g, 340 mmol) was taken in 20 ml acetic acid and 40 ml acetic anhydride (400 mmol), stirred at 50° C. until all cyanoacetic acid was solved. Phenyl urea (33.05 g, 247.5 mmol) was added and the mixture was stirred at 95° C. for 60 minute under LC-MS (Liquid Chromatography coupled with Mess Spectrometer) control of the reaction progress. After cooling down to room temperature, dilution with 20 ml 2-propanol and storing at 4° C. for 2 h, solids were separated by filtration, washed with cold 2-propanol and dried under high vacuum giving 40.06 g of white solids (82.6%).

1. temperatureAfter cooling down to room temperature
2. customsolids were separated by filtration
3. washwashed with cold 2-propanol
4. customdried under high vacuum