反应详情

To N-{3-[(4-cyano-1H-pyrrolo[2,3-b]pyridin-3-yl)-hydroxy-methyl]-2,4-difluoro-phenyl}-4-trifluoromethyl-benzenesulfonamide (6, 15 mg, 0.030 mmol) dissolved in 0.2 mL of tetrahydrofuran, Dess-Martin periodinane (13.8 mg, 0.0324 mmol) was added. The reaction mixture was stirred at room temperature for one hour. The reaction mixture was poured into saturated sodium thiosulfate, the organic layer separated and washed with brine, then dried over sodium sulfate and filtered. The filtrate was concentrated under vacuum and the resulting material was purified by silica gel column chromatography, eluting with ethyl acetate and hexane. The appropriate fractions were combined and the solvent removed under vacuum to provide the desired compound (P-0001, 4 mg). MS (ESI) [M−H+]−=505.5.

1. customthe organic layer separated
2. washwashed with brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationThe filtrate was concentrated under vacuum
6. customthe resulting material was purified by silica gel column chromatography
7. washeluting with ethyl acetate and hexane
8. customthe solvent removed under vacuum