反应详情

温度

0 °C

3-Chloro-4,5-dimethoxypyridazine (17.0 g) and morpholine (59.0 mL) were stirred at 100° C. for 2 hr, and cooled to 0° C. To the reaction mixture was added phenyl isocyanate (73.8 mL) at 0° C., and the mixture was stirred at the same temperature for min. and diluted with ethyl acetate. The resulting byproduct N-phenylmorpholine-4-carboxamide was removed by filtration. The filtrate was concentrated, and purified by silica gel column chromatography (ethyl acetate/hexane→methanol/ethyl acetate) to give the title compound (9.61 g).

1. customThe resulting byproduct N-phenylmorpholine-4-carboxamide was removed by filtration
2. concentrationThe filtrate was concentrated
3. custompurified by silica gel column chromatography (ethyl acetate/hexane→methanol/ethyl acetate)