反应详情

Dess-Martin periodinane (2.26 g, 5.33 mmol) was added in portions to a solution of (5-bromo-1-methyl-1H-pyrazol-4-yl)(4,6-dichloropyrimidin-5-yl)methanol (C25) (1.20 g, 3.55 mmol) in chloroform (30 mL), and the mixture was stirred for 2 hours. After filtration, the filtrate was concentrated in vacuo, diluted with ethyl acetate (300 mL), washed with saturated aqueous sodium hydrogen sulfite solution (3×150 mL), and washed with saturated aqueous sodium carbonate solution. The organic layer was dried over magnesium sulfate, filtered, and concentrated under reduced pressure. Purification using silica gel chromatography (Eluent: 5:1 heptane/ethyl acetate) provided the product. Yield: 1.16 g, 3.45 mmol, 97%. LCMS m/z 337.1 (M+1). 1H NMR (400 MHz, CDCl3) δ 3.97 (s, 3H), 7.92 (s, 1H), 8.90 (s, 1H).

1. filtrationAfter filtration
2. concentrationthe filtrate was concentrated in vacuo
3. additiondiluted with ethyl acetate (300 mL)
4. washwashed with saturated aqueous sodium hydrogen sulfite solution (3×150 mL)
5. washwashed with saturated aqueous sodium carbonate solution
6. dry with materialThe organic layer was dried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customPurification
10. customprovided the product