反应详情

4-Fluoro-3-hydroxy-benzonitrile (15 g), 2-bromo-1-[4-(3,4-dichloro-benzyloxy)-phenyl]-ethanone (45 g), and potassium carbonate 45 g) were suspended together in 630 mL acetone with stirring. The mixture continued to stir for 18 hours, then was concentrated to dryness. The solid residue was taken up in 500 mL diethyl ether and stirred 1.5 h, then 1 L water was added and stirred vigorously an additional 3 hours. The solid product was collected by filtration and washed with 200 mL diethyl ether three times. It was then dissolved in THF, filtered to remove any remaining inorganic salt, and evaporated again to dryness. After drying under vacuum 18 h, 48 g of desired product was obtained (quantitative). 1H NMR (400 MHz, DMSO-d6): 7.97 (d, 2H), 7.66 (d, 1H), 7.45 (m, 2H), 7.46 (m, 3H), 7.16 (d, 2H), 5.72 (s, 2H), 5.25 (s, 2H).

1. stirringto stir for 18 hours
2. concentrationwas concentrated to dryness
3. stirringstirred 1.5 h
4. addition1 L water was added
5. stirringstirred vigorously an additional 3 hours
6. filtrationThe solid product was collected by filtration
7. washwashed with 200 mL diethyl ether three times
8. dissolutionIt was then dissolved in THF
9. filtrationfiltered
10. customto remove any remaining inorganic salt
11. customevaporated again to dryness
12. customAfter drying under vacuum 18 h