Ethyl chloroformate → 9-ethoxycarbonylaminomethyl-2-chloro-4-(o-chlorophenyl)-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine

반응식

[NH2:1][CH2:2][C:3]1[N:7]2[C:8]3[S:22][C:21]([Cl:23])=[CH:20][C:9]=3[C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])=[N:11][CH2:12][C:6]2=[N:5][N:4]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:30]([O:32][C:33](Cl)=[O:34])[CH3:31]>O1CCOCC1>[CH2:30]([O:32][C:33]([NH:1][CH2:2][C:3]1[N:7]2[C:8]3[S:22][C:21]([Cl:23])=[CH:20][C:9]=3[C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])=[N:11][CH2:12][C:6]2=[N:5][N:4]=1)=[O:34])[CH3:31]

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실험 절차

0.6 g of 9-aminomethyl-2-chloro-4-(o-chlorophenyl)-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine are dissolved in 15 ml of absolute dioxane. 1.5 g of potassium carbonate are suspended in the solution and 0.18 g of chloroformic acid ethyl ester added with stirring. After 3 hours, the solid material is filtered off from the solution. The residue obtained after evaporation of the filtrate is recrystallized from ethyl acetate containing active carbon, to yield 9-ethoxycarbonylaminomethyl-2-chloro-4-(o-chlorophenyl)-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine.