反应详情

N-(tert-Butyl)-2-(difluoromethyl)-5-(5-phenyl-4-((pyridin-2-ylmethyl)amino) pyrrolo[2,1-f][1,2,4]triazin-2-yl)pyridine-3-sulfonamide (0.520 g, 0.923 mmol) was dissolved in CH2Cl2 (4 mL). Then TFA (1.0 0 mL, 13.0 mmol) was added and stirred at RT for 16 h. The volatile components were removed under reduced pressure and the resulting residue was diluted with 10% NaHCO3 (25 mL). The reaction mixture was extracted with EtOAc (2×25 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The resulting residue was purified by preparative HPLC (Condition B-96 as described in general methods) to afford 2-(difluoromethyl)-5-(5-phenyl-4-((pyridin-2-ylmethyl)amino)pyrrolo[2,1-f][1,2,4]triazin-2-yl)pyridine-3-sulfonamide (0.140 g, 29.9%) as a pale yellow solid. LCMS Condition B-78: retention time 2.29 min, [M+1]=508.2. HPLC Condition B-31: retention time 8.65 min, purity 98.6%. 1H NMR (400 MHz, DMSO-d6) δ ppm 4.95 (d, J=4.8 Hz, 2H), 6.87 (d, J=2.8 Hz, 1H), 7.28-7.62 (m, 9H), 7.75-7.82 (m, 1H), 7.99 (d, J=2.4 Hz, 1H), 8.17 (s, 2H), 8.38-8.40 (m, 1H), 9.09 (d, J=1.6 Hz, 1H), 9.67 (d, J=2.0 Hz, 1H).

1. customThe volatile components were removed under reduced pressure
2. additionthe resulting residue was diluted with 10% NaHCO3 (25 mL)
3. extractionThe reaction mixture was extracted with EtOAc (2×25 mL)
4. dry with materialThe combined organic extracts were dried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe resulting residue was purified by preparative HPLC (Condition B-96 as described in general methods)