HCID 11845250, Verbindung → HCID 11847134, Verbindung
Reaktionsgleichung
[N+:1]([C:4]1[CH:24]=[CH:23][C:7]([CH2:8][O:9][C:10]([N:12]2[CH2:17][CH2:16][N:15]3[N:18]=[C:19]([CH2:21][OH:22])[CH:20]=[C:14]3[CH2:13]2)=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2]>O=[Mn]=O.C(Cl)(Cl)Cl.CO>[N+:1]([C:4]1[CH:24]=[CH:23][C:7]([CH2:8][O:9][C:10]([N:12]2[CH2:17][CH2:16][N:15]3[N:18]=[C:19]([CH:21]=[O:22])[CH:20]=[C:14]3[CH2:13]2)=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2]Komponenten
4
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
MnO2 (activated) (84.2 g) was added to the CHCl3-MeOH (95:5, 253 mL) solution of 2-hydroxymethyl-6,7-dihydro-4H-pyrazolo[1,5-a]pyrazine-5-carboxylic acid 4-nitrobenzyl ester (8.42 g), and the mixture was refluxed for 1 h under a nitrogen atmosphere. The reaction mixture was filtered through a pad of Celite. Silica-gel (20 g) was added to the filtrate and the solvent was removed under reduced pressure to give the silica-gel coating with crude reactant. The above silica-gel was adsorbed to silica-gel column chromatography and the column was eluted with CHCl3-MeOH (49/1 to 19/1). The titled compound was obtained as yellow crystals (2.82 g, 34%).