反应详情

26.4 g (0.1 mol) of 2-acetyl-3-(2',2'-dichlorovinyl)-4-ethyl-γ-valerolactone were dissolved in 100 ml of dioxane. Technical grade hypochlorite solution was then added dropwise at 20-30° C. in an amount such that a total of 0.5 mol of hypochlorite had been added. The mixture was heated to the boil for a further 3-4 hours, any hypochlorite still present was destroyed with sodium bisulphite solution and the mixture was adjusted to pH 1 with 25% strength sulphuric acid. It was then extracted with methylene chloride and the organic phase was subjected to fractional distillation. 16.7 g (75% of theory) of 3-(2',2'-dichlorovinyl)-4-ethyl-γ-valerolactone of boiling point 160°-165° C./20 mm Hg were obtained. Refractive index: nD20 :1.5012.

1. additionhad been added
2. temperatureThe mixture was heated to the boil for a further 3-4 hours
3. customany hypochlorite still present was destroyed with sodium bisulphite solution
4. extractionIt was then extracted with methylene chloride
5. distillationthe organic phase was subjected to fractional distillation