反应详情

With ice-bath cooling under argon, 4-(4-pyridyl)-2(1H)-pyrimidinone (13.45 g, 77.7 mmol) and thionyl chloride (92 ml) were combined. N,N-Dimethylformamide (13.2 ml, 170.5 mmol) was added slowly and the mixture was heated to reflux for 1 h. It was evaporated and co-distilled with toluene. At 0° C., water was added to the remainder, then 10% ammonium hydroxide until neutral followed by extraction with dichloromethane. Drying of the organic solution was followed by evaporation and the resultant solid was recrystallized from acetone. MS (m/z): 192.1,194.0 (M+H)+; C9H6ClN3 requir. 191.6.

1. temperatureWith ice-bath cooling under argon
2. temperaturethe mixture was heated
3. temperatureto reflux for 1 h
4. customIt was evaporated
5. additionAt 0° C., water was added to the remainder
6. extraction10% ammonium hydroxide until neutral followed by extraction with dichloromethane
7. customDrying of the organic solution
8. customwas followed by evaporation
9. customthe resultant solid was recrystallized from acetone