反应详情

温度

120 °C

Copper(I)iodide (11.8 mg, 0.062 mmol) was added to a stirred suspension of 2-phenoxymethyl-6H-imidazo[1,2-c]pyrimidin-5-one (50 mg, 0.21 mmol), 4-fluoroiodobenzene (72.5 mg, 0.41 mmol), K2CO3 (57 mg, 0.41 mmol) and N,N′-dimethylethylenediamine (0.011 mL, 0.1 mmol) in toluene (1 mL) in a sealed tube. The mixture was stirred at 120° C. for 16 hours. The mixture was filtered through a pad of diatomaceous earth and then the solvent was evaporated in vacuo. The crude product was purified by flash column chromatography (silica; AcOEt in DCM with a gradient of 0/100 to 30/70). The desired fractions were collected and evaporated in vacuo to yield 6-(4-fluoro-phenyl)-2-phenoxymethyl-6H-imidazo[1,2-c]pyrimidin-5-one (45 mg, 65% yield) as a white solid. 1H NMR (500 MHz, CDCl3) 8 ppm 5.20 (s, 2H), 6.70 (d, J=7.8 Hz, 1H), 6.98 (t, J=7.2 Hz, 1H), 7.03 (d, J=8.1 Hz, 2H), 7.12 (d, J=7.8 Hz, 1H), 7.19-7.25 (m, 2H), 7.27-7.34 (m, 2H), 7.38-7.45 (m, 2H), 7.83 (s, 1H).

1. filtrationThe mixture was filtered through a pad of diatomaceous earth
2. customthe solvent was evaporated in vacuo
3. customThe crude product was purified by flash column chromatography (silica
4. customThe desired fractions were collected
5. customevaporated in vacuo