反应详情

25% NaOMe/methanol solution (92 μL) was added to an MeOH (2 mL) solution of methyl 2-chloro-6-phenylpyridine-4-carboxylate (1100 mg), and stirred at room temperature for 2 hours. Further, 25% NaOMe/methanol solution (92 μL) was added to it, and stirred under heat with refluxing for 2 hours and 30 minutes. DMA (3 mL) was added to it, and stirred overnight at 130° C., then 25% NaOMe/methanol solution (92 μL) was added to it, and stirred at 130° C. for 7 hours. With cooling with ice, diluted hydrochloric acid was added to it, the formed precipitate was taken out through filtration, washed with water, dried, and purified through reversed-phase high-performance liquid chromatography [acetonitrile/water+0.11% trifluoroacetic acid] to obtain the title compound as a white powder.

1. stirringstirred
2. temperatureunder heat
3. temperaturewith refluxing for 2 hours and 30 minutes
4. stirringstirred overnight at 130° C.
5. stirringstirred at 130° C. for 7 hours
6. additionwas added to it
7. filtrationthe formed precipitate was taken out through filtration
8. washwashed with water
9. customdried
10. custompurified through reversed-phase high-performance liquid chromatography [acetonitrile/water+0.11% trifluoroacetic acid]