反应详情

Sodium hydride 80% dispersion in oil (0.057 g) was added portionwise to a solution of 2,4-dioxo-5-phenyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine (0.40 g) in dry dimethylformamide (15 ml). The reaction mixture was cooled to 0° and stirred for 30 min, then a solution of 3-methyl-1-bromobutane (0.23 ml) in dry dimethylformamide (4 ml) was added and stirring continued for 2 h. The reaction mixture was then diluted with water (100 ml), extracted with ethyl acetate (3×100 ml), washed with brine (2×50 ml), dried and concentrated in vacuo to give an oil which was purified by flash -chromatography (eluting with CH-EA 60:40) to give the title compound as a white solid (0.44 g). T.l.c. CH-EA (1:1), Rf=0.36.

1. temperatureThe reaction mixture was cooled to 0°
2. stirringstirring
3. waitcontinued for 2 h
4. extractionextracted with ethyl acetate (3×100 ml)
5. washwashed with brine (2×50 ml)
6. customdried
7. concentrationconcentrated in vacuo
8. customto give an oil which
9. customwas purified by flash -chromatography (eluting with CH-EA 60:40)