反应详情

温度

25 °C

To a stirred solution of LAH (3.01 g, 79.10 mmol) in THF (80 mL) at 0° C. was added 2,2-dimethyl-4H-benzo[1,4]oxazin-3-one (7.00 g, 39.5 mmol) in portions and stirred the reaction mixture at 25° C. for 1 h and then 50° C. for 3 h. Reaction mixture was quenched by the addition cold saturated sodium sulfate solution and it was filtered through celite and extracted with DCM (100 mL×2), washed with brine (50 mL), dried over sodium sulfate, concentrated to give 2,2-dimethyl-3,4-dihydro-2H-benzo[1,4]oxazine (6.09 g), which was used as such for the next reaction without purification

1. wait50° C. for 3 h
2. customReaction mixture
3. customwas quenched by the addition cold saturated sodium sulfate solution and it
4. filtrationwas filtered through celite
5. extractionextracted with DCM (100 mL×2)
6. washwashed with brine (50 mL)
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated