反应详情

温度

110 °C

A mixture of 12-chloro-4-[3-methyl-1-(2,2,2-trifluoroethyl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene (50.0 mg, 0.130 mmol), 1-methyl-4-(pyrrolidin-2-yl)piperidine (30.0 mg, 0.178 mmol), Pd(P-t-Bu3)2 (6.00 mg, 0.0120 mmol), and NaOt-Bu (40.0 mg, 0.412 mmol) in toluene (20.0 mL) in a seal tube was stirred at 110° C. for 3 h. After concentration, the residue was purified by reverse phase Combiflash eluting with a 0-40% gradient of CH3CN in 0.5% NH4HCO3 to afford 253 (8 mg, 12% yield) as white solid. LCMS (ESI): RT=4.70 min, m/z: 517.3 [M+H+]. 1H-NMR (500 MHz, DMSO-d6) δ 9.03 (s, 1H), 7.66 (s, 1H), 5.85 (s, 1H), 5.70 (dd, J=8.5 Hz, J=23.5 Hz, 2H), 4.46-4.43 (m, 4H), 4.06 (s, 1H), 3.38 (s, 1H), 3.26 (s, 1H), 2.09 (s, 3H), 1.95 (s, 9H), 1.84-1.72 (m, 2H), 1.52-1.34 (m, 3H), 1.19-1.12 (m, 2H)

1. concentrationAfter concentration
2. customthe residue was purified by reverse phase Combiflash
3. washeluting with a 0-40% gradient of CH3CN in 0.5% NH4HCO3