[C:1]1([CH:7]([S:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][N+:11]=2[O-:16])[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(O)(=[O:19])C.OO>[O-][W]([O-])(=O)=O.[Na+].[Na+].O>[C:1]1([CH:7]([S:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][N+:11]=2[O-:16])=[O:19])[CH3:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1To a mixture of 23.2 g (0.1 mole) of 2-(1-phenylethylthio)pyridine N-oxide, 0.2 g of sodium tungstate, and 60 ml of glacial acetic acid were added 10 ml (0.1 mole) of 30% hydrogen peroxide over approximately 0.5 hours. The mixture exothermed somewhat to about 65° C. After completion of the reaction, the reaction mixture was poured slowly into 800 ml of vigorously stirred cold water. A solid separated out and was filtered off and washed with 15 ml of cold ethanol. The solid was air dried, melting point 130–130.5° C. Yield 14.5 g or 59%. An infrared spectrum confirmed the structure.
Wird geladen…
