反应详情

210 mg of 7-allyl-6-methoxy-1,4-dihydrobenz[d][1,3]oxazin-2-one was dissolved in 6 ml of N,N-dimethylformamide. Thereafter, 46 mg of 60% sodium hydride was added to the reaction solution while cooling on ice. The obtained mixture was then stirred at room temperature for 20 minutes. Thereafter, while cooling on ice, 0.20 g of iodomethane was added to the reaction solution. The obtained mixture was then stirred at room temperature for 2 hours. Thereafter, the reaction solution was diluted with ethyl acetate and then washed with water and a saturated sodium chloride aqueous solution. The organic layer was dried over magnesium sulfate and then concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate), so as to obtain 207 mg of the subject compound.

1. temperaturewhile cooling on ice
2. additionwas added to the reaction solution
3. stirringThe obtained mixture was then stirred at room temperature for 2 hours
4. washwashed with water
5. dry with materialThe organic layer was dried over magnesium sulfate
6. concentrationconcentrated under a reduced pressure
7. customThe residue was purified by silica gel column chromatography (hexane-ethyl acetate)