反应详情

温度

50 °C

To a stirred solution of 6-(5-bromo-2-chloro-benzyl)-3,4-dihydro-2H-benzo[1,4]oxazine (8.0 g, 23.66 mmol) in DMF (35 mL) was added potassium carbonate (6.53 g, 36.0 mmol), benzyl bromide (4.33 mL, 35.50 mmol) and heated to 50° C. for 8 h. Reaction mixture was cooled to room temperature, quenched by the addition of water (50 mL), extracted with ethyl acetate (3×20 mL). The organic layer was washed with water (50 mL), brine (50 mL), dried over sodium sulfate, concentrated and purified by silica gel column chromatography to furnish 4-benzyl-6-(5-bromo-2-chloro-benzyl)-3,4-dihydro-2H-benzo[1,4]oxazine (7.0 g).

1. customReaction mixture
2. temperaturewas cooled to room temperature
3. customquenched by the addition of water (50 mL)
4. extractionextracted with ethyl acetate (3×20 mL)
5. washThe organic layer was washed with water (50 mL), brine (50 mL)
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated
8. custompurified by silica gel column chromatography