反应详情

温度

130 °C

A mixture of 1-{4-[1-(2-hydroxyethyl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaen-12-yl}ethan-1-one (115 mg, 0.290 mmol) and DMF-DMA (69 mg, 0.58 mmol) in xylenes (10 mL) was stirred at 130° C. for 48 h under nitrogen atmosphere. The mixture was then concentrated under reduced pressure, the residue was purified by reverse phase Combiflash eluting with a 0-40% gradient of CH3CN in 0.3% NH4HCO3 to give (2E)-3-(dimethylamino)-1-{4-[1-(2-hydroxyethyl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaen-12-yl}prop-2-en-1-one (120 mg, 90% yield). LCMS (ESI) m/z: 395.1 [M+H+].

1. concentrationThe mixture was then concentrated under reduced pressure
2. customthe residue was purified by reverse phase Combiflash
3. washeluting with a 0-40% gradient of CH3CN in 0.3% NH4HCO3