反应详情

To a solution of 4-[(phenylmethyl)oxy]-1H-indazole (D1) (280 mg, 1.25 mmol) in dichloromethane (20 mL) was added {3,5-difluoro-4-[(phenylmethyl)oxy]phenyl}boronic acid {DE patent application 4236105} (660 mg, 2.50 mmol), pyridine (0.202 mL, 2.50 mmol), copper acetate (340 mg, 1.88 mmol) and powdered 4A molecular sieves (500 mg). The reaction mixture was stirred at room temperature in the presence of air for 6 days. Celite was added to the mixture then the mixture was filtered through a pad of celite and then the filtrate was washed with water. After separation of the layers, the aqueous phase was re-extracted with dichloromethane. The combined organic layers were dried over magnesium sulphate, filtered and concentrated. The product was purified by silica gel chromatography eluting with 5-100% ethyl acetate in hexane to yield the title compound (D35 (257 mg).

1. additionCelite was added to the mixture
2. filtrationthe mixture was filtered through a pad of celite
3. washthe filtrate was washed with water
4. customAfter separation of the layers
5. extractionthe aqueous phase was re-extracted with dichloromethane
6. dry with materialThe combined organic layers were dried over magnesium sulphate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe product was purified by silica gel chromatography
10. washeluting with 5-100% ethyl acetate in hexane