反应详情

温度

110 °C

A mixture of 8-(4-bromo-2-fluoro-phenylamino)-imidazo[1,5-a]pyridine-7-carboxylic acid methyl ester (235 mg, 0.65 mmol), copper (I) iodide (6 mg, 0.03 mmol), sodium iodide (195 mg, 1.3 mmol) and trans-N,N′-dimethyl-1,2-cyclohexane diamine (0.01 mL, 0.06 mmol) in 1,4-dioxane (1.0 mL) was heated at 110° C. for 26 hours under an argon atmosphere. The reaction mixture was cooled to room temperature, diluted with methanol and loaded onto an Isolute® SCX-2 cartridge (10 g). The cartridge was then washed with methanol and the desired product was subsequently eluted using 2M NH3 in MeOH. The eluent was collected and concentrated to give a residue. The residue was subjected to flash chromatography (Si-PPC, gradient 0% to 20%, ethyl acetate in dichloromethane) to afford the title compound as a pale yellow solid (182 mg, 67%). LCMS (method B): RT=3.45 min, [M+H]+=412.

1. temperatureThe reaction mixture was cooled to room temperature
2. washThe cartridge was then washed with methanol
3. washthe desired product was subsequently eluted
4. customThe eluent was collected
5. concentrationconcentrated
6. customto give a residue