反应详情

To a slurry of 10% palladium on carbon (0.15 g) in methanol(12 mL) were added 6-fluoro-3-(2-methyl-pyridin-3-yl)-2-[2-(2-methyl-thiazol-4-yl)-vinyl]-3 H-quinazolin-4-one (0.075 g, 0.198 mmol) and ammonium formate (1.2 g, 19 mmol). The mixture was refluxed overnight, cooled and filtered through celite. The pad was washed with methanol. The filtrate was concentrated. The residue was partitioned between chloroform and water. The phases were separated and the aqueous layer was extracted with chloroform. The combined organic phase was washed with water and brine, dried over magnesium sulfate, and concentrated to afford 0.035 g (47%) of 6-fluoro-3-(2-methyl-pyridin-3-yl)-2-[2-(2-methyl-thiazol-4-yl)-ethyl]-3H-quinazolin-4-one as a white solid.

1. temperatureThe mixture was refluxed overnight
2. temperaturecooled
3. filtrationfiltered through celite
4. washThe pad was washed with methanol
5. concentrationThe filtrate was concentrated
6. customThe residue was partitioned between chloroform and water
7. customThe phases were separated
8. extractionthe aqueous layer was extracted with chloroform
9. washThe combined organic phase was washed with water and brine
10. dry with materialdried over magnesium sulfate
11. concentrationconcentrated