反应详情

温度

110 °C

To a mixture of 3-bromo-N-[2-[3-(2,2-dimethylpropanoylamino)-4-methyl-phenyl]imidazo[2,1-f]pyridazin-6-yl]benzamide (0.126 g, 0.25 mmol), Ethyl acrylate (0.272 mL, 2.5 mmol), palladium(II) acetate (2.8 mg, 0.01 mmol), tri(o-tolyl)phosphine (0.0152 g, 0.05 mmol) in DMF (1.45 mL) is added DIPEA (0.174 mL, 1 mmol). The mixture is degassed with N2 then sealed and heated at 110° C. for 18 hours. The reaction mixture is cooled, saturated aqueous NaHCO3 (50 mL) added and extracted with EtOAc (×3). Organic layers are combined and washed with water, NaHCO3, brine, then dried, concentrated and purified by silica gel chromatography (0-100% EtOAc in Hexanes) to give the title compound (0.040 g). LCMS (m/z)=526.6 [M+H]+, tR=2.92 min.

1. customThe mixture is degassed with N2
2. customthen sealed
3. temperatureThe reaction mixture is cooled
4. additionsaturated aqueous NaHCO3 (50 mL) added
5. extractionextracted with EtOAc (×3)
6. washwashed with water, NaHCO3, brine
7. customdried
8. concentrationconcentrated
9. custompurified by silica gel chromatography (0-100% EtOAc in Hexanes)