反应详情

A 1.62 ml quantity of pyridine was dissolved in 60 ml of dichloroethane. To the solution was added 0.89 g of aluminum chloride powder, and the mixture was refluxed with heating for 15 minutes. Then to the mixture were added 2.20 g of 2,6-di-tert-butyl-1,4-benzoquinone and 0.95 g of aminopyrazine, and the mixture was refluxed under heating for 17.5 hours. The reaction mixture was cooled to room temperature and filtered through a Celite pad and the insoluble materials were washed there with dicloromethane. The filtrate was concentrated, and the resulting crude product was purified by silica gel column chromatography (eluent: diethyl ether-hexane=3:7), giving 1.73 g of Compound 1a.

1. temperaturethe mixture was refluxed
2. temperaturewith heating for 15 minutes
3. temperaturethe mixture was refluxed
4. temperatureunder heating for 17.5 hours
5. filtrationfiltered through a Celite pad
6. washthe insoluble materials were washed there with dicloromethane
7. concentrationThe filtrate was concentrated
8. customthe resulting crude product was purified by silica gel column chromatography (eluent: diethyl ether-hexane=3:7)