Methanol → HCID 46203371, Verbindung

Reaktionsgleichung

[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[C:15]([CH3:17])([CH3:16])[C:14](=[O:18])[N:13]([CH:19]3[CH2:24][CH2:23][N:22]([S:25]([C:28]4[CH:29]=[C:30]([CH:34]=[CH:35][CH:36]=4)[C:31]([OH:33])=[O:32])(=[O:27])=[O:26])[CH2:21][CH2:20]3)[N:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].S(=O)(=O)(O)O.[CH3:42]O>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[C:15]([CH3:17])([CH3:16])[C:14](=[O:18])[N:13]([CH:19]3[CH2:24][CH2:23][N:22]([S:25]([C:28]4[CH:29]=[C:30]([CH:34]=[CH:35][CH:36]=4)[C:31]([O:33][CH3:42])=[O:32])(=[O:26])=[O:27])[CH2:21][CH2:20]3)[N:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

Komponenten

Edukt 3

HCID 887Methanol

HCID 1118Sulfuric Acid

HCID 46203370HCID 46203370, Verbindung

Produkt 1

HCID 46203371HCID 46203371, Verbindung

Versuchsvorschrift

0.5 g 3-({4-[3-(3,4-Dimethoxyphenyl)-4,4-dimethyl-5-oxo-4,5-dihydro-1H-pyrazol-1-yl]piperidin-1-yl}sulfonyl)benzoic acid (compound described in example 25) are suspended in 20 ml of methanol, 0.2 ml concentrated sulfuric acid are added, and the reaction mixture is heated to reflux for 24 h. The solvent is removed under reduced pressure, the residue is taken up in DCM, the organic phase is washed with aqueous sodium carbonate solution (5%) and dried over MgSO4. The solvents are evaporated under reduced pressure and the crude product is crystallized from DCM and diethyl ether to yield the title compound.