反应详情

温度

0 °C

POCl3 (5.6 mL, 61.3 mmol) was added dropwise to a solution of 1-(4-fluorophenyl)-3-methoxypyrazin-2(1H)-one in DMF (30 mL) with stirring at 0° C. followed by heating at 90° C. for 1.5 hours. The residue was cooled to 0° C., quenched by adding saturated sodium acetate solution, extracted with CH2Cl2, washed with water, dried over MgSO4, and concentrated. The crude was purified by silica gel flash column chromatography (0.7% MeOH in CH2Cl2) to afford 3.52 g (64%) of the desired product. LRMS (ESI pos) m/e 224.9, 227.0 (M+1, Cl pattern).

1. temperatureby heating at 90° C. for 1.5 hours
2. temperatureThe residue was cooled to 0° C.
3. customquenched
4. additionby adding saturated sodium acetate solution
5. extractionextracted with CH2Cl2
6. washwashed with water
7. dry with materialdried over MgSO4
8. concentrationconcentrated
9. customThe crude was purified by silica gel flash column chromatography (0.7% MeOH in CH2Cl2)