反应详情

A suspension of 1.04 g (3.0 mmol) of 3-(5-chloromethyl-1,2,4-oxadiazol-3-yl)-8-fluoro-5-methyl-5,6-dihydro-4H-imidazo[1,5-a]-[1,4]benzodiazepin-6-one in 10 ml of N,N-dimethylformamide was treated with 1.27 ml (9.0 mmol) of diisopropylamine. After stirring at room temperature for 18 hrs. the solution obtained was concentrated and the residue was taken up in 10 ml of water and stirred in an ultrasound bath for 2 hrs. The crystals were filtered off under suction and dissolved in methylene chloride, and the solution was dried with sodium sulfate, is filtered and evaporated. The crude material was chromatographed on silica gel (ethyl acetate), dissolved in acetonitrile and acidified with ethereal hydrochloric acid. The solution was again evaporated and the residue was recrystallized from acetonitrile. After drying in a vacuum there were obtained 542 mg (38%) of 3-(5-diisopropylaminomethyl-1,2,4-oxadiazol-3-yl)-8-fluoro-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one as white crystals of m.p. 173°-178° (dec.).

1. customthe solution obtained
2. concentrationwas concentrated
3. stirringstirred in an ultrasound bath for 2 hrs
4. filtrationThe crystals were filtered off under suction
5. dissolutiondissolved in methylene chloride
6. dry with materialthe solution was dried with sodium sulfate
7. filtrationis filtered
8. customevaporated
9. customThe crude material was chromatographed on silica gel (ethyl acetate)
10. dissolutiondissolved in acetonitrile
11. customThe solution was again evaporated
12. customthe residue was recrystallized from acetonitrile
13. customAfter drying in a vacuum there