反应详情

To {5-[hydroxy-(7H-pyrrolo[2,3-d]pyrimidin-5-yl)-methyl]-pyridin-2-yl}-(6-methoxy-pyridin-3-ylmethyl)-carbamic acid tert-butyl ester (72, 0.189 g, 0.409 mmol) in 4.0 mL of dichloromethane, Dess-Martin periodinane (0.208 g, 0.490 mmol) was added. The reaction was stirred at room temperature for 1 hour, then poured into aqueous potassium carbonate and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material was purified by silica gel column chromatography, eluting with methanol and dichloromethane. Appropriate fractions were combined and the solvents removed under vacuum to provide the desired compound (73, 66 mg). 1H NMR was consistent with the compound structure.

1. extractionextracted with ethyl acetate
2. dry with materialThe organic layer was dried over sodium sulfate
3. filtrationfiltered
4. concentrationthe filtrate concentrated under vacuum
5. customThe resulting material was purified by silica gel column chromatography
6. washeluting with methanol and dichloromethane
7. customthe solvents removed under vacuum