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
PROCEDURE
实验过程
4.5 g (14 mmol) of 8-(5,6-dichloro-1H-benzo[d]imidazol-2-yl)-3,4-dihydro-2H-benzo[b][1,4]oxazine (compound 1a) obtained in Example 5 was dissolved in 100 mL of dimethylformamide. 1.3 g (7 mmol) of 4-(2-chloroethyl)morpholine, 0.58 g (3.5 mmol) of potassium iodide and 0.97 g (7 mmol) of K2CO3 were added thereto, followed by irradiation of microwave at 110° C. for 10 min. The reaction mixture was concentrated under reduced pressure, followed by dilution with ethyl acetate. The resulting product was washed with distilled water and saturated sodium chloride solution, followed by drying over magnesium sulfate and concentrating under reduced pressure. The resulting residue was subjected to column chromatography (ethyl acetate/hexane=1/1) to obtain the title compound (2.8 g, yield: 91%).
WORKUP
后处理
- customfollowed by irradiation of microwave at 110° C. for 10 min
- concentrationThe reaction mixture was concentrated under reduced pressure
- washThe resulting product was washed with distilled water and saturated sodium chloride solution
- dry with materialby drying over magnesium sulfate
- concentrationconcentrating under reduced pressure