反应详情

tert-Butyl {(1R,2R)-2-[({4-[6-(difluoromethoxy)pyrazolo[1,5-a]pyrimidin-3-yl]-5-ethylthiophen-2-yl}carbonyl)amino]-3,3-difluorocyclohexyl}carbamate (0.037 g, 0.064 mmol) was dissolved in dichloromethane (0.639 mL) and trifluoroacetic acid (0.250 mL, 3.24 mmol) was added. The reaction was stirred at room temperature for 2 h. 5N NaOH (aq) was added and extracted 3× with dichloromethane. The organic layers were combined, dried with sodium sulfate, filtered, and concentrated. The material was purified by column chromatography (0-5% MeOH/DCM) to give the title compound. LRMS (APCI) calc'd for (C20H21F4N5O2S) [M+H]+, 472.1; found 472.1. 1H NMR (CD3OD, 500 MHz) δ 9.04 (d, J=2.4, 1H), 8.59 (d, J=2.4, 1H), 8.35 (s, 1H), 8.13 (s, 1H), 6.97 (t, J=72.5, 1H), 3.24 (s, 1H), 3.02 (q, J=7.5, 2H), 2.15 (s, 1H), 1.48-1.99 (m, 4H), 1.32 (t, 3H), 1.00-1.18 (m, 2H).

1. extractionextracted 3× with dichloromethane
2. dry with materialdried with sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customThe material was purified by column chromatography (0-5% MeOH/DCM)