Hydrochloric Acid → HCID 70937947, compound

Participants

Reaction Steps

Sodium borohydride (26.4 mg, 0.698 mmol) was added in 3 portions over 4 h to a solution of methyl 2-[5-[(3R,5S)-5-(tert-butoxycarbonylamino)-6-(2,5-difluorophenyl)tetrahydrothiopyran-3-yl]-4,6-dihydropyrrolo[3,4-c]pyrazol-2-yl]acetate (13.2 mg, 0.025 mmol) in methanol (0.25 mL). After an additional 15 min, 2N HCl (0.1 mL, 0.1 mmol) was added and the resulting suspension was stirred at room temperature for 5 min. Filtration of the suspension and purification by reverse-phase HPLC was followed by preparative thin layer plate chromatography (1×500 micron PTLC plate), developed with a 90:10 mixture of methylene chloride/(10:1 EtOH/concentrated ammonium hydroxide). The appropriate uv active band was removed, eluted with a 90:10 mixture of methylene chloride/(10:1 EtOH/concentrated ammonium hydroxide) and evaporated to give the title compound as a white solid. MS: 499.2 [M+1]

Provenance & Evidence