反应详情

温度

160 °C

In a 500 ml three necked round bottom flask was charged 4,4-dimethyl-cyclohexanol (100 g, 0.78 mol) and heated up to 160° C., while adding over 4 hours tBuOOtBu (11.4 g, 0.08 mol) and ethylacrylate (39.2 g, 0.39 mol). 10 minutes after the end of the addition, the mixture was cooled to 50° C. and lights were distilled off. Then, 30% w/w aqueous NaOH (61 g) and MTBE (200 g) were added. Stirring was continued during the night at 40° C. and the aqueous phase was separated. The aqueous phase was re-extracted four times with MTBE (200 g). Afterwards, MTBE (200 g) was added to the aqueous phase, and the pH adjusted to 1 with 50% w/w aqueous H2SO4. The organic phase was washed with water and concentrated to yield 49.4 g of crude 8,8-dimethyl-1-oxa-spiro[4.5]decan-2-one (GC purity: 96.3%).

1. addition10 minutes after the end of the addition
2. temperaturethe mixture was cooled to 50° C.
3. distillationlights were distilled off
4. additionThen, 30% w/w aqueous NaOH (61 g) and MTBE (200 g) were added
5. customwas continued during the night at 40° C.
6. customthe aqueous phase was separated
7. extractionThe aqueous phase was re-extracted four times with MTBE (200 g)
8. additionAfterwards, MTBE (200 g) was added to the aqueous phase
9. washThe organic phase was washed with water
10. concentrationconcentrated