反应详情

To 2-methyl-propane-1-sulfonic acid {2,4-difluoro-3-[hydroxy-(4-methyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-methyl]-phenyl}-amide (77, 99 mg, 0.24 mmol) in 2 mL of tetrahydrofuran, Dess-Martin periodinane (112 mg, 0.265 mmol) is added and the reaction is stirred at room temperature for 2 hours. The reaction is poured into saturated aqueous sodium thiosulfate along with some sodium bicarbonate solid and extracted with ethyl acetate. The organic layer is washed with water, then brine, and dried with sodium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material is purified by silica gel column chromatography, eluting with ethyl acetate and dichloromethane. Appropriate fractions are combined and concentrated under vacuum to provide the desired compound (P-1003, 28 mg). MS (ESI) [M+H+]+=409.3.

1. extractionextracted with ethyl acetate
2. washThe organic layer is washed with water
3. dry with materialbrine, and dried with sodium sulfate
4. filtrationfiltered
5. concentrationthe filtrate concentrated under vacuum
6. customThe resulting material is purified by silica gel column chromatography
7. washeluting with ethyl acetate and dichloromethane
8. concentrationconcentrated under vacuum