Trifluoroacetic acid → HCID 22029751, Verbindung
Reaktionsgleichung
C(OC([N:8]1[CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH:9]1[CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[N:28]1[C:36]2[C:35](=[O:37])[N:34]([CH3:38])[C:33](=[O:39])[N:32]([CH3:40])[C:31]=2[N:30]=[CH:29]1)=O)(C)(C)C.[F:41][C:42]([F:47])([F:46])[C:43]([OH:45])=[O:44]>>[F:41][C:42]([F:47])([F:46])[C:43]([OH:45])=[O:44].[CH3:40][N:32]1[C:31]2[N:30]=[C:29]3[N:28]([C:36]=2[C:35](=[O:37])[N:34]([CH3:38])[C:33]1=[O:39])[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=1[CH2:21][CH:9]1[CH2:10][NH:11][CH2:12][CH2:13][N:8]31Komponenten
3
Versuchsvorschrift
2-[2-(1,3-dimethyl-2,6-dioxo-1,2,3,6-tetrahydropurin-7-yl)benzyl]piperazine-1,4-dicarboxylic acid di-tert-butyl ester (0.055 g) was dissolved in trifluoroacetic acid (0.5 ml), the mixture was stirred for 30 minutes, and the solvent was removed by distillation at reduced pressure. The residue was dissolved in N,N-dimethylformamide, and N-chlorosuccinimide (0.025 g) was added to the solution. The mixture was stirred at room temperature for 14 hours, 1,8-diazabicyclo-[5,4,0]-7-undecene (0.050 ml) was added thereto, and was further stirred for 1 hour. After removing the solvent by distillation at reduced pressure, the residue was purified by HPLC with a reversed phase column using water-acetonitrile-trifluoroacetic acid system as elution solvent to give 0.0079 g of the title compound.