反应详情

温度

150 °C

To a solution of (3-bromo-6-fluoro-pyridin-2-ylmethyl)-(4-methoxy-benzyl)-3-phenyl-urea (644 mg, 1.5 mmol, 1.0 equiv) and N,N-diisopropylethylamine (500 μL, 2.9 mmol, 2.0 equiv) in DMF (15 mL) was added CuI (331 mg, 1.7 mmol, 1.2 equiv) and the reaction mixture was heated at 150° C. for 5 h. The reaction mixture was cooled, H2O was added and the product was extracted with EtOAc. The organic phase was washed with dilute NH4OH, brine, dried (MgSO4), filtered and concentrated under reduced pressure. The crude product was purified by column chromatography (SiO2, eluted with petrol—EtOAc 0-50%) to afford 6-fluoro-3-(4-methoxy-benzyl)-1-phenyl-3,4-dihydro-1H-pyrido[3,2-d]pyrimidin-2-one (300 mg). MS: [M+H]+=364.

1. temperatureThe reaction mixture was cooled
2. extractionthe product was extracted with EtOAc
3. washThe organic phase was washed with dilute NH4OH, brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude product was purified by column chromatography (SiO2, eluted with petrol—EtOAc 0-50%)