反应详情

温度

100 °C

17.7 grams (0.065 mole) of the product of Example 1 was dissolved in 60 mls of dry dimethylformamide along with 0.25 grams of potassium hydroxide and 7.5 grams (0.085 mole) of ethylene carbonate. The mixture was heated to 100° C. and maintained for 2 hours until no carbon dioxide was liberated. The solution was then heated at 110° C. for 30 minutes. The solution was filtered and the dimethylformamide was distilled under reduced pressure with a mechanical pump. The solid was dried in a drying pistol using xylene as the solvent. The residual solid was recrystallized from ethyl alcohol to give 10.4 grams (50%) yield of a solid melting at 197°-198° C. Calculated for C19H15N3O2, C, 71.9; H, 4.8; N, 13.2. Found: C, 71.7; H, 4.71; N, 13.5. The infrared spectra showed the OH group at 2.9μ, the nitrile band at 4.5μ, and the carbonyl band at 6.0μ. The NMR confirmed that the product was the desired material.

1. temperatureThe solution was then heated at 110° C. for 30 minutes
2. filtrationThe solution was filtered
3. distillationthe dimethylformamide was distilled under reduced pressure with a mechanical pump
4. customThe solid was dried in a drying pistol
5. customThe residual solid was recrystallized from ethyl alcohol