反应详情

The a 3-liter round-bottomed flask provided with a stirrer , thermometer, condenser and dropping funnel, there are added 353 g (2.3 mol) of 2-tert. butyl-cyclohexanone 14 g of anhydrous sodium acetate and 1.17 liters of methylene chloride. 370 g of ca. 40% peracetic acid are added at room temperature while cooling. The mixture is held first at room temperature for 20 hours with stirring and then for a further 48 hours under reflux temperature. After cooling, the mixture is poured on to ice, the layers are separated and the organic layer washed with an iron sulphate solution and then with water until a neutral reaction is obtained. The solvent is distilled off and the crude lactone distilled, there being obtained 274 g (70.3%) of the Σ-lactone of 6-hydroxy-7,7-dimethylcaprylic acid of boiling point 134° C/12 mm Hg; melting point 54°-58° C.

1. customThe a 3-liter round-bottomed flask provided with a stirrer
2. customthermometer, condenser and dropping
3. temperaturewhile cooling
4. temperaturefor a further 48 hours under reflux temperature
5. temperatureAfter cooling
6. additionthe mixture is poured on to ice
7. customthe layers are separated
8. washthe organic layer washed with an iron sulphate solution
9. customwith water until a neutral reaction
10. customis obtained
11. distillationThe solvent is distilled off
12. distillationthe crude lactone distilled