反应详情

温度

40 °C

To a solution of 12-bromo-4-iodo-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene (1.0 g, 2.6 mmol) in dry DMF (20 mL) was added hydrochloric acetimidamide (266 mg, 2.81 mmol), Pd(OAc)2 (58 mg, 0.26 mmol), and Xantphos (305 mg, 0.520 mmol). The reaction mixture was stirred at 40° C. for 3 h under carbon monoxide atmosphere. LCMS indicated complete conversion. Acetic acid (40 mL) and hydrochloric (2-methoxypropyl)hydrazine (577 mg, 5.20 mmol) were added, the resultant mixture was stirred at 100° C. for 1 h. After concentration, the residue was purified by silica gel chromatography eluting with DCM/methanol (100:1) to give 12-bromo-4-[1-(2-methoxypropyl)-3-methyl-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene (707 mg, 65% yield) as white solid. LCMS (ESI) m/z: 418.3 [M+H+].

1. concentrationAfter concentration
2. customthe residue was purified by silica gel chromatography
3. washeluting with DCM/methanol (100:1)