反应详情

温度

100 °C

To a solution of 12-chloro-N-[(1E)-(dimethylamino)methylidene]-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaene-4-carboxamide (0.25 mmol, 80 mg) in acetic acid (3 mL) was added hydrochloric isopropylhydrazine (0.50 mmol, 5 mg). The mixture was stirred at 100° C. for 1 h under nitrogen atmosphere. After removal of the solvent, the residue was purified by reverse phase combiflash eluting with a 0-50% gradient of CH3CN in 0.3% NH4HCO3 to give 12-chloro-4-[1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaene (50 mg, 61% yield). LCMS (ESI) m/z: 331.1 [M+H+]. 1H NMR (500 MHz, DMSO-d6): δ 9.29 (s, 1H), 8.02 (s, 1H), 7.94 (s, 1H), 7.24 (s, 1H), 5.86 (t, J=13.5 Hz, 1H), 4.68-4.65 (m, 2H), 4.61-4.59 (m, 2H), 1.49 (d, J=6.5 Hz, 6H)

1. customAfter removal of the solvent
2. customthe residue was purified by reverse phase combiflash
3. washeluting with a 0-50% gradient of CH3CN in 0.3% NH4HCO3