反应详情

A solution of (R)-2-(4-(5-cyanothiophen-2-yl)-2-(2,4-dimethoxybenzyl)-7-fluoro-3-oxo-2,3-dihydro-1H-pyrrolo[3,4-c]pyridin-6-ylamino)-4-methylpentanamide (68 mg, 0.126 mmol) in TFA (2 mL) was heated to 65° C. for 3 h. After removal of the solvent, the resulting crude material was reconstituted in MeOH/DCM (3.0 mL) and purified via preparative HPLC eluting with water (0.05% TFA) and ACN (40%, 0.035% TFA). The collected fractions were combined and the solvent was removed via rotary evaporation to yield the title compound (8.3 mg, 17%). 1H NMR (500 MHz, DMSO-d6) δ ppm 0.86-0.96 (m, 6 H), 1.53-1.62 (m, 1 H), 1.67-1.88 (m, 2 H), 4.45 (s, 2 H), 4.50-4.57 (m, 1 H), 6.96-7.06 (m, 1 H), 7.32-7.54 (m, 2 H), 7.86-8.02 (m, 1 H), 8.61 (s, 1 H), 9.00-9.15 (m, 1 H). [M+H] calc'd for C18H18FN5O2S, 388; found, 388.

1. customAfter removal of the solvent
2. custompurified via preparative HPLC
3. washeluting with water (0.05% TFA) and ACN (40%, 0.035% TFA)
4. customthe solvent was removed via rotary evaporation