反应详情

112 g of 2-methylcyclohexanone and 500 ml carbon tetrachloride are mixed in a three neck flask and 90 ml of thionyl chloride in 150 ml of carbon tetrachloride are added dropwise in the course of 60 minutes, under vigorous stirring while keeping the temperature at about 15° with a water bath. Stirring is maintained for a further 2 hours. The reaction medium is then washed three times with dilute hydrochloric acid, twice with a saturated solution of sodium bicarbonate and finally with a saturated solution of sodium chloride. The organic phase is separated, dried over sodium sulphate and the solvent is evaporated off under reduced pressure. The dry residue of 2-methyl-2-chlorocyclohexanone weighing about 180 g is purified by fractional distillation. The main fraction boils at 85°-90° (20 mm Hg); nD25 =1.4672.

1. additionare added dropwise in the course of 60 minutes
2. customat about 15°
3. stirringStirring
4. temperatureis maintained for a further 2 hours
5. washThe reaction medium is then washed three times with dilute hydrochloric acid
6. customThe organic phase is separated
7. dry with materialdried over sodium sulphate
8. customthe solvent is evaporated off under reduced pressure
9. distillationThe dry residue of 2-methyl-2-chlorocyclohexanone weighing about 180 g is purified by fractional distillation