[N:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[N:5]=[C:4]([NH2:12])[CH2:3][C:2]=1[NH2:13].CS(C)=O.[CH3:18][N:19]1[CH2:24][CH2:23]N[CH2:21][CH2:20]1>C1(C)C=CC=CC=1>[CH3:18][N:19]1[CH2:24][CH2:23][N:12]([C:4]2[CH2:3][C:2]([N:13]3[CH2:21][CH2:20][N:19]([CH3:18])[CH2:24][CH2:23]3)=[N:1][C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=3[N:5]=2)[CH2:21][CH2:20]13H-[1,5]Benzodiazepine-2,4-diamine (32.50 g, 160 mmol, 86%) was added to a solution of dimethyl sulfoxide (220 ml), toluene (220 ml) and 1-methylpiperazine (165 ml). The mixture was heated for 16 h at 120° C. After cooling the product precipitated. It was filtered off and washed with isopropyl ether (80 ml) to give 40.1 g (74%) of the title compound as off-white needles. The second crop was obtained by adding isopropyl ether (410 ml) to the filtrate. The mixture was allowed to stand overnight at 4° C., the crystallised product was filtered off to give additional 4.25 g (8%) of the title compound. For analytical purposes the product was recrystallised from ethyl acetate.
Wird geladen…
