反应详情

温度

110 °C

When a mixture of 0.50 mole of ethyl diphenylphosphinite, 0.55 mole of n-butyraldehyde, and 0.25 mole of urea in 150 ml of chlorobenzene is warmed at 110° C for 3 hr, there is only a slow reaction. The mixture is cooled to room temperature and 0.25 mole of acetic acid is addded dropwise in ~10 minutes. The temperature increases to 65° during this addition; the urea dissolves and then a white solid product separates. The addition of another 0.25 mole of acetic acid causes no additional heat of reaction. The reaction mixture is warmed at 65°-80° for 9.5 hr and filtered, giving 44.4g. Recrystallization from ethylene glycol gives 26.5g of a white solid: mp 241°-244°; 31P nmr (CF3CO2H) -44.4 ppm; ms M+ = 316 (theory 316).

1. customa slow reaction
2. temperatureThe mixture is cooled to room temperature
3. temperatureThe temperature increases to 65° during this addition
4. temperatureno additional heat of reaction
5. temperatureThe reaction mixture is warmed at 65°-80° for 9.5 hr
6. filtrationfiltered
7. customgiving 44.4g
8. customRecrystallization from ethylene glycol