[C:1]1([N:7]2[C:11]([SH:12])=[N:10]C=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:13]C(C)=O.CI.[C:19](=[O:22])([O-])[O-].[Na+].[Na+]>O>[C:1]1([N:7]2[C:11]([S:12][CH3:13])=[N:10][C:19]([OH:22])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1An amount of 23.2 g of 1-phenyl-5-mercapto-1,2,4-triazole, M.P. 220°C, is placed into 50 ml of acetone, 50 ml of water and 10 ml of methyliodide. An addition is then made in portions, within 15 minutes, of 21 g of sodium carbonate, and, after completion of the addition, stirring continued for 1 hour at 30°C. The acetone is evaporated off, and the solution acidified with dilute hydrochloric acid. The precipitated product is filtered off, and recrystallised from 250 ml of ethanol to obtain 1-phenyl-5-methylmercapto-3-hydroxy-1,2,4-triazole in the form of white crystals having a melting point of 176°-177°C.
Loading…
