反应详情

温度

90 °C

A mixture of tert-butyl (1S,2R)-2-(4-chloro-2-(2,4-dimethoxybenzyl)-7-fluoro-3-oxo-2,3-dihydro-1H-pyrrolo[3,4-c]pyridin-6-ylamino)cyclohexylcarbamate (200 mg, 0.364 mmol) and hydrobromic acid in HOAc (10 mL) was stirred at 90° C. for 6 h. The mixture was concentrated under reduced pressure, and the resulting crude material was reconstituted in MeOH (1.0 mL) and was purified via preparative HPLC eluting with water (0.05% TFA) and ACN (15-30% gradient, 0.035% TFA). The collected fractions were combined and ACN was removed via rotary evaporation. The resulting aqueous solution was neutralized with saturated aqueous NaHCO3, washed with EtOAc (2×200 mL), dried over Na2SO4, and filtered. The organic phase was stripped to dryness via rotary evaporation to yield the title compound (38 mg, 30%). [M+H] calc'd for C13H16BrFN4O, 343; found, 343.

1. concentrationThe mixture was concentrated under reduced pressure
2. customwas purified via preparative HPLC
3. washeluting with water (0.05% TFA) and ACN (15-30% gradient, 0.035% TFA)
4. customACN was removed via rotary evaporation
5. washwashed with EtOAc (2×200 mL)
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. customThe organic phase was stripped to dryness via rotary evaporation