反应详情

温度

60 °C

To a stirred solution of 3,4-dihydro-2H-benzo[1,4]oxazine (4.0 g, 29.6 mmol) in DMF (20 ml) was added potassium carbonate (10.22 g, 74.0 mmol). After stirring for five min. Iodo-ethane (3.5 ml, 44.4 mmol) was added and heated to 60° C. for overnight. Reaction mixture was cooled to room temperature, quenched by the addition of water (20 ml), extracted with ethyl acetate (3×25 ml). The organic layer was washed with water (30 ml), brine (30 ml), dried over sodium sulfate, concentrated and purified by silica gel column chromatography to furnish 4-ethyl-3,4-dihydro-2H-benzo[1,4]oxazine (2.7 g).

1. customReaction mixture
2. temperaturewas cooled to room temperature
3. customquenched by the addition of water (20 ml)
4. extractionextracted with ethyl acetate (3×25 ml)
5. washThe organic layer was washed with water (30 ml), brine (30 ml)
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated
8. custompurified by silica gel column chromatography