反应详情

Into a 500 ml reaction flask equipped with reflux head, thermometer and stirrer is added 50 g of 40% sulfuric acid and 50 g of anhydrous isopropyl alcohol. The resulting mixture is heated to reflux and 1,3,3-trimethyl-1-cyclohexene-4-ethanol, prepared according to Example II (50 g) (fraction 2 according to Example II) is added slowly to the reaction mass while maintaining the temperature thereof at 86°-88° C. The addition takes place over a period of one hour. At the end of the addition of the cyclohexene derivative, the reaction mass is cooled to room temperature and water is added. The reaction mass now exists in two phases. The phases are separated and the organic phase is washed with aqueous sodium carbonate and saturated sodium chloride. The organic phase is then distilled using a microdistillation set-up (micro Vigreux column) yielding the following fractions:

1. customInto a 500 ml reaction flask
2. customequipped
3. temperaturewith reflux head
4. temperatureThe resulting mixture is heated
5. temperatureto reflux
6. additionis added slowly to the reaction mass
7. temperaturewhile maintaining the temperature
8. customat 86°-88° C
9. additionThe addition
10. customof one hour
11. customThe phases are separated
12. washthe organic phase is washed with aqueous sodium carbonate and saturated sodium chloride
13. distillationThe organic phase is then distilled
14. customyielding the following fractions