Hydrochloric Acid → HCID 66811089, Verbindung

Reaktionsgleichung

[F:1][C:2]1[CH:7]=[C:6]([C:8](=[N:18]O)[C:9]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)=[O:10])[CH:5]=[CH:4][N:3]=1.C(O)(C)C.[ClH:24]>[Pd]>[ClH:24].[NH2:18][CH:8]([C:6]1[CH:5]=[CH:4][N:3]=[C:2]([F:1])[CH:7]=1)[C:9]([C:11]1[CH:12]=[CH:13][C:14]([F:17])=[CH:15][CH:16]=1)=[O:10]

Komponenten

Versuchsvorschrift

With gentle heating, 22b (5.0 g; 19 mmol) was dissolved in HCl-containing isopropanol (IsOH/HCl-saturated IsOH 1+1, 60 ml). The yellowish solution was cooled to room temperature and transferred into a two-necked flask (100 ml). Pd—C 10% (1.5 g) was introduced into the initial charge. The reaction vessel was evacuated using an oil pump and H2 was then introduced via a gas inlet capillary (4×). At room temperature, the suspension was shaken in a closed three-necked flask under an atmosphere of H2 (240 strokes/min) until no more starting material could be detected by thin-layer chromatography (6.5 h). The catalyst was filtered off. The filtration residue was washed with plenty of methanol (about 800 ml). The combined filtrates were concentrated and the solid-amorphous residue was dried on an oil pump. The crude product was used without further purification for the next reaction step.