反应详情

To a solution of tert-butyl 6-((3R,4R)-3-(tert-butoxycarbonylamino)tetrahydro-2H-pyran-4-ylamino)-7-fluoro-4-(3-methylisothiazol-5-yl)-3-oxo-1H-pyrrolo[3,4-c]pyridine-2(3H)-carboxylate (5.5 mg, 9.76 μmol) in DCM (2.0 mL) was added TFA (2.0 mL, 26.0 mmol). The reaction mixture was stirred at RT for 1 h, and concentrated in vacuo. The resulting crude material was reconstituted in DMF and purified via preparative HPLC eluting with water (0.05% TFA) and ACN (55-80% gradient, 0.035% TFA). The collected fractions were combined and the ACN was removed via rotary evaporation. The resulting aq solution was neutralized with saturated aq NaHCO3, washed with EtOAc (2×50 mL), dried over anhydrous Na2SO4, filtered, and the organic phase stripped to dryness via rotary evaporation. The residue was recrystallized from THF/hexane to give a TFA salt of the title compound. [M+H] calc'd for C16H18FN5O2S, 364; found, 364.

1. concentrationconcentrated in vacuo
2. custompurified via preparative HPLC
3. washeluting with water (0.05% TFA) and ACN (55-80% gradient, 0.035% TFA)
4. customthe ACN was removed via rotary evaporation
5. washwashed with EtOAc (2×50 mL)
6. dry with materialdried over anhydrous Na2SO4
7. filtrationfiltered
8. customthe organic phase stripped to dryness via rotary evaporation
9. customThe residue was recrystallized from THF/hexane