Triacetoxyperiodinane → HCID 44469404, compound

Participants

Reaction Steps

To propane-1-sulfonic acid 2,4-difluoro-3-[hydroxy-(7H-pyrrolo[2,3-d]pyrimidin-5-yl)-methyl]-phenyl-amide (P-0001, 0.150 g, 0.392 mmol), 3 mL of tetrahydrofuran was added, followed by Dess-Martin periodinane (0.166 g, 0.392 mmol). The reaction was allowed to stir at room temperature for 1 hour, then the reaction was extracted with ethyl acetate and 5:1 saturated sodium bicarbonate:saturated sodium thiosulfate. The organic layer was dried with magnesium sulfate, filtered, and the filtrate concentrated under vacuum. The resulting material was purified by silica gel column chromatography eluting with a gradient of 1 to 5% methanol in dichloromethane. Appropriate fractions were combined and concentrated under vacuum to give the desired compound (P-0002, 110 mg). MS(ESI)[M+H+]+=381.2. LC/MS indicated 97.0% purity.

Provenance & Evidence