[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.[CH3:9][C:10]([C:13]([CH2:15][N:16]1[N:20]=[CH:19][N:18]=[CH:17]1)=[O:14])([CH3:12])[CH3:11].C=O.N1CCCC[CH2:24]1>C1(C)C=CC=CC=1.O.C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:24][CH:15]([N:16]2[CH:17]=[N:18][CH:19]=[N:20]2)[C:13](=[O:14])[C:10]([CH3:9])([CH3:11])[CH3:12])=[CH:4][CH:3]=1A mixture of 72.5 g (0.5 mol) of 4-chlorothiophenol, 100.2 g (0.6 mol) of 1,2,4-triazol-1-yl-pinacolin, 18 g (0.6 mol) of paraformaldehyde, 15 g of acetic acid and 5 ml of piperidine in 600 ml of toluene was heated under reflux in a water separator. After the water has been separated off, the reaction solution was washed with water, dried over sodium sulphate, filtered, and concentrated in vacuo. The oily residue was chromatographed over a silica gel column (mobile phase: chloroform). 45 g (28% of theory) of 1-(4-chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pentan -3-one of melting point 67° C. were obtained.
読み込み中…