反应详情

Sodium hydride 80% dispersion in oil (0.07 g) was added portionwise to a solution of 2,4-dioxo-5-phenyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine (0.5 g) in DMF (50 ml). The reaction mixture was stirred for 30 min, then a solution of 1-adamantylmethyl methanesulfonate (0.537 g) in DMF (3 ml) was added. The reaction mixture was stirred at 120° for 7 h and at 23° for 15 h, then concentrated. The residue was diluted with ethyl acetate (100 ml) washed with brine (2×30 ml) and water (50 ml), dried and concentrated "in vacuo". The crude product was purified by flash chromatography (eluting with CH-EA 1:1) to give the title compound as a white foam (0.15 g). T.l.c. CH-EA (1:1), Rf =0.42.

1. stirringThe reaction mixture was stirred at 120° for 7 h and at 23° for 15 h
2. concentrationconcentrated
3. additionThe residue was diluted with ethyl acetate (100 ml)
4. washwashed with brine (2×30 ml) and water (50 ml)
5. customdried
6. concentrationconcentrated "in vacuo"
7. customThe crude product was purified by flash chromatography (eluting with CH-EA 1:1)