反应详情

温度

80 °C

To a solution of 8-(2,4-dimethylphenyl)-2-methyl-2H-1,4-benzoxazin-3(4H)-one (300 mg, 1.12 mmol) in N,N-dimethylformamide (5 ml) was added sodium hydride (43 mg, 1.68 mmol). After the mixture was stirred at 80° C. for 30 min, 4-bromoheptane (804 mg, 4.49 mmol) was added. The mixture was stirred at 80° C. for 18 h and diluted with water. The aqueous solution was extracted with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate and concentrated under vacuum. The residue was purified by column chromatography eluting with 5% ethyl acetate/n-hexane to afford 186 mg (30%) of the title compound.

1. stirringThe mixture was stirred at 80° C. for 18 h
2. extractionThe aqueous solution was extracted with ethyl acetate
3. washThe extract was washed with brine
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under vacuum
6. customThe residue was purified by column chromatography
7. washeluting with 5% ethyl acetate/n-hexane