Diisopropyl Ether → 4,5-Diacetoxy-2-pyridinecarbonyl chloride hydrochloride

반응식

P(Cl)(Cl)(Cl)(Cl)[Cl:2].[C:7]([O:10][C:11]1[C:16]([O:17][C:18](=[O:20])[CH3:19])=[CH:15][N:14]=[C:13]([C:21]([OH:23])=O)[CH:12]=1)(=[O:9])[CH3:8].C(OC(C)C)(C)C>C(Cl)Cl>[ClH:2].[C:7]([O:10][C:11]1[C:16]([O:17][C:18](=[O:20])[CH3:19])=[CH:15][N:14]=[C:13]([C:21]([Cl:2])=[O:23])[CH:12]=1)(=[O:9])[CH3:8]

참가 물질

실험 절차

To a suspension of phosphorus pentachloride (4.6 g) in methylene chloride (40 ml) was added 4,5-diacetoxy-2-pyridinecarboxylic acid (4.5 g) at -20° C. with stirring. The stirring was continued for an hour at -18°~-12° C. To the reaction mixture was add%d diisopropyl ether (80 ml) below 0° C. The resulting precipitates were collected by filtration, washed with diisopropyl ether and dried over phosphorus pentoxide to give 4,5-diacetoxy-2-pyridinecarbonyl chloride hydrochloride (5.15 g).