反应详情

温度

110 °C

To a solution of N-ethyl-N-(2-fluoro-4-iodobenzyl)ethanamine (1.72 g, 5.60 mmol) in dioxane (50 mL) was added 3,5-dimethyl-pyridone (0.69 g, 5.60 mmol), N,N′-dimethyl ethane-1,2-diamine (0.20 g, 2.24 mmol), CuI (0.21 g, 1.12 mmol) and potassium phosphate (2.38 g, 11.20 mmol) under N2. The reaction mixture was heated at 110° C. for 9 h, then cooled to rt and poured into CH2Cl2 (200 mL). The mixture was filtered, and the filtrate was washed with water (200 mL×3) and brine (200 mL). The organic phase was concentrated in vacuo. The residue was purified by a silica gel column chromatography (CH2Cl2/MeOH (V/V)=10:1) to give the title compound as a yellow solid (0.23 g, 14%). The compound was characterized by the following spectroscopic data:

1. temperaturecooled to rt
2. filtrationThe mixture was filtered
3. washthe filtrate was washed with water (200 mL×3) and brine (200 mL)
4. concentrationThe organic phase was concentrated in vacuo
5. customThe residue was purified by a silica gel column chromatography (CH2Cl2/MeOH (V/V)=10:1)