反应详情

温度

70 °C

A mixture of 12-bromo-13-methyl-4-[1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene (1.0 g, 2.6 mmol), tributyl(1-ethoxyvinyl)stannane (1.2 mL), Pd(PPh3)4 (90 mg, 7.8 mmol), and LiCl (328 mg, 7.8 mmol) in dry THF (10 mL) was stirred at 70° C. for 48 h under nitrogen atmosphere. KF (100 mL, 0.16 M) was added and the mixture was further stirred at room temperature for 1 h. The solid was filtered off. The filtrate was concentrated to give the crude product, which was purified by reverse phase Combiflash eluting with a 0-50% gradient of CH3CN in 0.3% NH4HCO3 to afford 12-(1-ethoxyethenyl)-13-methyl-4-[1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene (660 mg, 68% yield). LCMS (ESI) m/z: 380.2 [M+H+].

1. stirringthe mixture was further stirred at room temperature for 1 h
2. filtrationThe solid was filtered off
3. concentrationThe filtrate was concentrated
4. customto give the crude product, which
5. customwas purified by reverse phase Combiflash
6. washeluting with a 0-50% gradient of CH3CN in 0.3% NH4HCO3