反应详情

To 4-acetylpyridine (23 mL) in 350 mL toluene was added 55 mL N,N-dimethylformamide dimethyl acetal. The solution was refluxed for 3 hours and allowed to stir at ambient temperature overnight. An additional 33 mL N,N-dimethylformamide dimethyl acetal of was added. After refluxing for 7 hours, the mixture was concentrated to leave an orange solid. This material was treated with diethyl ether. The resulting yellow solid was collected by vacuum filtration. A total of 25.85 g (71% yield) yellow solid was obtained. 1H NMR (CDCl3) was consistent with the desired structure. LC/MS indicated a single peak with a M+1 molecular ion of m/z 177.1 by positive ESI (electrospray ionization mass spectrometry).

1. temperatureThe solution was refluxed for 3 hours
2. temperatureAfter refluxing for 7 hours
3. concentrationthe mixture was concentrated
4. customto leave an orange solid
5. filtrationThe resulting yellow solid was collected by vacuum filtration