Dimethylamine → HCID 15907985, Verbindung

Reaktionsgleichung

[C:1]([NH:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[S:30])[NH:13][C:14]2[CH:27]=[C:26]([Cl:28])[C:17]([O:18][CH2:19][CH2:20]OS(C)(=O)=O)=[C:16]([Cl:29])[CH:15]=2)=[CH:7][CH:6]=1)(=[O:3])[CH3:2].[CH3:31][NH:32][CH3:33]>O1CCCC1.C(OCC)(=O)C>[Cl:28][C:26]1[CH:27]=[C:14]([NH:13][C:12](=[S:30])[NH:11][C:8]2[CH:9]=[CH:10][C:5]([NH:4][C:1](=[O:3])[CH3:2])=[CH:6][CH:7]=2)[CH:15]=[C:16]([Cl:29])[C:17]=1[O:18][CH2:19][CH2:20][N:32]([CH3:33])[CH3:31]

Komponenten

Versuchsvorschrift

To a solution of methanesulfonic acid 2-{4-[3-(4-acetylamino-phenyl)-thioureido]-2,6-dichlorophenoxy}-ethyl ester (0.33 g) in tetrahydrofuran (6 mL) is added aqueous dimethyl-amine (8.8 M, 0.5 mL) and the mixture is stirred at room temperature for 5 days. The reaction mixture is then diluted with ethyl acetate, then washed with saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate. After removal of the solvent tinder reduced pressure the residue is chromatographed over silica gel (pure methanol is used as the eluant). Pooled product containing fractions are evaporated tinder reduced pressure and the residue is recrystallized from acetonitrile to provide the desired product as a white powder.