反应详情

7-Methoxy-4-methyl-4H-benzo[1,4]oxazin-3-one (13.07 g, 0.68 mol) was added to 100 mL dry THF, and the reaction mixture was refluxed under nitrogen. Borane-dimethyl sulfide (13.6 mL, 0.136 mol) was added dropwise over one hour, and the reaction mixture was allowed to reflux for two hours. The reaction mixture was cooled and then quenched by addition of 50 mL of 10% aqueous HCl. Precipitate was removed by filtration, and the liquid was concentrated under reduced pressure to give 11.17 g of 7-Methoxy-4-methyl-3,4-dihydro-2H-benzo[1,4]oxazine. (M+H)=180.

1. temperaturethe reaction mixture was refluxed under nitrogen
2. temperatureto reflux for two hours
3. temperatureThe reaction mixture was cooled
4. customquenched by addition of 50 mL of 10% aqueous HCl
5. customPrecipitate was removed by filtration
6. concentrationthe liquid was concentrated under reduced pressure