HRID1747798
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
3-Chloro-4,5-dimethoxypyridazine (17.0 g) and morpholine (59.0 mL) were stirred at 100° C. for 2 hr and the mixture was 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 30 min and diluted with ethyl acetate. The resulting 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).
WORKUP
后处理
- customThe resulting N-phenylmorpholine-4-carboxamide was removed by filtration
- concentrationThe filtrate was concentrated
- custompurified by silica gel column chromatography (ethyl acetate/hexane→methanol/ethyl acetate)