反应详情

To a suspension of 6-nitro-2H-1,4-benzoxazin-3(4H)-one (J. Med. Chem. 1989, 32, 1627-1630) (1 g, 5.7 mmol) in dry THF (20 ml) at 0° C. under argon, was added NaH (0.16 g, 5.7 mmol, 80% dispersion in mineral oil). A solution of 2-dimethylaminoethyl chloride (2.3 g, 20.8 mmol) in dry toluene (15 ml) was added and the reaction mixture heated under reflux for 19 hr. After cooling, water was added dropwise until effervescence had ceased, then the mixture was separated and the aqueous further extracted with EtOAc. The organic layers were combined, dried (Na2SO4) and evaporated under reduced pressure to give a pale brown solid (1.08 g, 79%).

1. temperaturethe reaction mixture heated
2. temperatureunder reflux for 19 hr
3. temperatureAfter cooling
4. customthe mixture was separated
5. extractionthe aqueous further extracted with EtOAc
6. dry with materialdried (Na2SO4)
7. customevaporated under reduced pressure