Ethyl formate → HCID 12234603, Verbindung
Reaktionsgleichung
[CH:1](OCC)=[O:2].[CH3:6][N:7]1[C:13]2[CH:14]=[CH:15][C:16]([Cl:18])=[CH:17][C:12]=2[CH:11]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[NH:10][CH2:9][C:8]1=[O:25]>ClC1C=CC=CC=1>[CH3:6][N:7]1[C:13]2[CH:14]=[CH:15][C:16]([Cl:18])=[CH:17][C:12]=2[CH:11]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[N:10]([CH:1]=[O:2])[CH2:9][C:8]1=[O:25]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
6 ml. of ethyl formate are added to a solution of 1.4 g. (5 mmoles) of 1-methyl-5-phenyl-7-chloro-1,3,4,5-tetrahydro-2H-1,4-benzodiazepine-2-one in 5 ml. of chlorobenzene, and the reaction mixture is maintained at the boiling point of the solvent for 3 hours. Thereafter the solvent is evaporated under reduced pressure, and the oily residue is solidified by treating it with 20 ml. of dry ether. 108 g. (68.6 %) of 1-methyl-4-formyl-5-phenyl-7-chloro-1,3,4,5-tetrahydro-2H-1,4-benzodiazepine-2-one are obtained; m.p.: 167°-169° C. The melting point does not change after recrystallization from ethanol. Rf2 = 0.5.