反应详情

温度

120 °C

A glass microwave reaction vessel was charged with (3R)-tert-butyl 3-(4-(5-(2,6-difluorophenyl)-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-3-yl)-6-(4-methoxybenzyloxy)pyrimidin-2-ylamino)piperidine-1-carboxylate (145 mg, 0.200 mmol) and TFA (1.5 mL, 19.47 mmol). The reaction was stirred and heated in a Initiator microwave reactor (Personal Chemistry, Biotage AB, Inc., Upssala, Sweden) at 120° C. for 20 min. then solvent was removed. The residue was purified with preparative HPLC (10-50% ACN in water with 0.1% TFA) to give (R)-6-(5-(2,6-difluorophenyl)-1H-indazol-3-yl)-2-(piperidin-3-ylamino)pyrimidin-4-ol (54.0 mg, 0.128 mmol, 64.1% yield) as a TFA salt. MS (ESI, pos. ion) m/z: 423 (M+1); 1H NMR (400 MHz, DMSO-d6) δ ppm 13.65 (1 H, br. s.), 8.59-8.71 (1 H, m), 8.41-8.56 (2 H, m), 7.73 (1 H, s), 7.41-7.55 (2 H, m), 7.17-7.32 (2 H, m), 6.87 (1 H, br. s.), 6.40 (1 H, br. s.), 4.18 (2 H, br. s.), 3.23 (1 H, d, J=10.4 Hz), 3.01-3.16 (2 H, m), 2.87 (1 H, q, J=10.0 Hz), 2.11 (1 H, d, J=13.1 Hz), 1.70-1.84 (1 H, m), 1.38-1.65 (2 H, m).

1. customA glass microwave reaction vessel
2. customsolvent was removed
3. customThe residue was purified with preparative HPLC (10-50% ACN in water with 0.1% TFA)