反应详情

温度

60 °C

A mixture of 13-(1-ethoxyethenyl)-4-[3-methyl-1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6,12-triazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaene (900 mg, 2.36 mmol) and 4-methylbenzenesulfonic acid (204 mg, 1.18 mmol) in acetone (20 mL) was stirred at 60° C. for 75 min. After removal of the solvent, the residue was purified by reverse phase Combi-flash eluting with a 23-27% gradient of CH3CN in 0.3% NH4HCO3 to give the desired product (650 mg, 74% yield) as a pale yellow solid. 1H NMR (500 MHz, DMSO-d6) δ 8.85 (s, 1H), 8.49 (s, 1H), 8.07 (s, 1H), 5.69 (m, 1H), 4.68-4.59 (m, 4H), 2.63 (s, 3H), 2.29 (s, 3H), 1.49 (s, 6H). LCMS m/z [M+H]+ 353.3

1. customAfter removal of the solvent
2. customthe residue was purified by reverse phase Combi-flash
3. washeluting with a 23-27% gradient of CH3CN in 0.3% NH4HCO3