Reaktionsgleichung
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[C:16]3[CH:17]=[C:18]4[O:23][CH2:22][O:21][C:19]4=[CH:20][C:15]=3[CH2:14][C:13]([CH3:24])=[N:12][N:11]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2].C(O)C.Cl.[BH4-].[Na+]>>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([C:10]2[C:16]3[CH:17]=[C:18]4[O:23][CH2:22][O:21][C:19]4=[CH:20][C:15]=3[CH2:14][CH:13]([CH3:24])[NH:12][N:11]=2)=[CH:8][CH:9]=1)([O-:3])=[O:2]Komponenten
Versuchsvorschrift
To a suspension of 5.0 g (15.5 mmol) of the known 1-(4-nitrophenyl-4-methyl-7,8-methylenedioxy-5H-2,3-benzodiazepine (French patent specification No. 85,09793) in 380 ml of ethanol first 22.5 ml (0.278 mol) of concentrated hydrochloric acid were added at constant stirring whereupon a solution was formed within a few minutes, then 11.5 g (0.3 mole) of sodium borohydride were charged into the solution portionwise during 30 minutes. Stirring was continued for 15 minutes, then the orange-coloured precipitate formed was filtered and extracted on the filter with 4×30 ml of chloroform. The combined chloroform filtrate was evaporated under reduced pressure, the crystalline residue was brought to a filter with 200 ml of distilled water, then washed with 3×20 ml of distilled Water and dried at 80°-100° C. to yield 4.90 g (97.2%) of the aimed product, m.p.: 162°-164° C.
Aufarbeitung
- additionTo a suspension of 5.0 g (15.5 mmol) of the
- additionwere added
- customwas formed within a few minutes
- stirringStirring
- customthe orange-coloured precipitate formed
- filtrationwas filtered
- extractionextracted on the
- filtrationfilter with 4×30 ml of chloroform
- customThe combined chloroform filtrate was evaporated under reduced pressure
- filtrationa filter with 200 ml of distilled water
- washwashed with 3×20 ml of distilled Water
- customdried at 80°-100° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-74c0bd76199a47d99802946c0194d6a5
- Quelldatensatz
- uspto-grants-1997_06
- Patentnummer
- US05639751
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