反应详情

温度

60 °C

8.3 g (0.074 mol) of 30% strength hydrogen peroxide were slowly added dropwise to a solution of 22.6 g (0.07 mol) of 1-(4-chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pentan-3-one (prepared as described in Example 1) in 100 ml of acetic acid and 2 drops of concentrated sulphuric acid. The reaction mixture was stirred for a further 18 hours at 60° C., and 8.3 g (0.074 mol) of 30% strength hydrogen peroxide were again added. The reaction mixture was then stirred for a further 18 hours at 80° C. Thereafter, the reaction solution was introduced into water, and the mixture was extracted with methylene chloride. The organic phase was dried over sodium sulphate, filtered, and concentrated in vacuo. The oily residue crystallized after being stirred with diisopropyl ether. 4.9 g (22% of theory) of 1-(4-chlorophenylsulphonyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pentan-3-one of melting point 134° C. were obtained.

1. stirringThe reaction mixture was then stirred for a further 18 hours at 80° C
2. extractionthe mixture was extracted with methylene chloride
3. dry with materialThe organic phase was dried over sodium sulphate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe oily residue crystallized
7. stirringafter being stirred with diisopropyl ether