反应详情

A mixture of 6-bromo-7-phenyl-1H-pyrido[2,3-b][1,4]oxazin-2(3H)-one (400 mg, 1.311 mmol), 1-fluoro-2-iodoethane (684 mg, 3.93 mmol) and potassium carbonate (544 mg, 3.93 mmol) in DMF (4 ml) was heated under stirring for 3 h. The reaction mixture was cooled down and diluted with water (20 ml), the resulted mixture was extracted with DCM (3×20 ml). The combined organic phase was washed with water, brine, dried over sodium sulfate, concentrated to give the crude material which was purified by column chromatography eluted with ethyl acetate/cyclohexane 0-40% to give product 0.21 g. 1H NMR (500 MHz, CDCl3): 7.39-7.48 (m, 5H), 4.89 (s, 2H), 4.77 (t, 1H), 4.67 (t, 1H), 4.21 (t, 1H), 4.16 (t, 1H), LCMS (Method D): RT=1.24 min, M+H+=353.0.

1. temperaturewas heated
2. temperatureThe reaction mixture was cooled down
3. extractionthe resulted mixture was extracted with DCM (3×20 ml)
4. washThe combined organic phase was washed with water, brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customto give the crude material which
8. customwas purified by column chromatography
9. washeluted with ethyl acetate/cyclohexane 0-40%