反应详情

To a suspension of 60% sodium hydride (1.6 g) in N,N-dimethylformamide (50 ml) was added 4-bromophenol (3.0 g) under a nitrogen atmosphere, the solution was stirred for 10 minutes at room temperature, then 1-(2-chloroethyl)azepane hydrochloride (4.0 g) and sodium iodide (in catalytic amounts) were sequentially added thereto followed by stirring overnight at 80° C. Water was added thereto followed by stirring, the solution was extracted with ethyl acetate, then sequentially washed with water and brine, and the solvent was evaporated in vacuo. The residue was purified by NH silica gel column chromatography (hexane-ethyl acetate system) to provide the title compound (5.0 g).

1. stirringby stirring overnight at 80° C
2. stirringby stirring
3. extractionthe solution was extracted with ethyl acetate
4. washsequentially washed with water and brine
5. customthe solvent was evaporated in vacuo
6. customThe residue was purified by NH silica gel column chromatography (hexane-ethyl acetate system)