反应详情

温度

100 °C

A mixture of 3-(1-chlorophthalazin-6-yl)-N-cyclopropyl-4-methylbenzamide (0.110 g, 326 μmol), 2,4,6-trimethylbenzeneboronic acid (53 mg, 326 μmol) and dichloro[1,1′-bis(diphenylphosphino)ferrocene]dichloride palladium(ii) dichloromethane adduct (12mg, 16 μmol) in 5 mL toluene/ethanol (4:1) was treated with 2 M potassium carbonate (488 μl, 977 μmol). The mixture was stirred at 100° C. under nitrogen and followed by MS for about 15 h. (product MS=422 (M+1)). The mixture was concentrated under vacuum and the crude product was purified via flash chromatography (silica gel) eluting with a gradient of 2% 2 M ammonia in MeOH/DCM to 6% 2 M ammonia in MeOH/DCM to give the title compound (80 mg). Found MS (ES+): 422(M+H)+.

1. concentrationThe mixture was concentrated under vacuum
2. customthe crude product was purified via flash chromatography (silica gel)
3. washeluting with a gradient of 2% 2 M ammonia in MeOH/DCM to 6% 2 M ammonia in MeOH/DCM