反应详情

温度

40 °C

To a solution of 12-chloro-4-iodo-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaene (2.0 g, 5.8 mmol) in dry DMF (20 mL) was added hydrochloric acetimidamide (595 mg, 6.30 mmol), Pd(OAc)2 (130 mg, 0.580 mmol), and Xantphos (695 mg, 1.2 mmol). The 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 (1.3 g, 12 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-chloro-4-[3-methyl-1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetra-deca1(14),2,4,10,12-pentaene (1.4 g, 71% yield) as a white solid. LCMS (ESI) m/z: 345.3 [M+H+].

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