Reaktionsgleichung
[CH3:1][C:2]1([CH3:9])[CH2:7][CH2:6][CH:5]([OH:8])[CH2:4][CH2:3]1.C(OOC(C)(C)C)(C)(C)C.C([O:22][C:23](=O)[CH:24]=[CH2:25])C>>[CH3:1][C:2]1([CH3:9])[CH2:7][CH2:6][C:5]2([O:8][C:23](=[O:22])[CH2:24][CH2:25]2)[CH2:4][CH2:3]1Komponenten
Reaktionsbedingungen
- Temperatur
- 160 °C
Versuchsvorschrift
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%).
Aufarbeitung
- addition10 minutes after the end of the addition
- temperaturethe mixture was cooled to 50° C.
- distillationlights were distilled off
- additionThen, 30% w/w aqueous NaOH (61 g) and MTBE (200 g) were added
- customwas continued during the night at 40° C.
- customthe aqueous phase was separated
- extractionThe aqueous phase was re-extracted four times with MTBE (200 g)
- additionAfterwards, MTBE (200 g) was added to the aqueous phase
- washThe organic phase was washed with water
- concentrationconcentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-233d41f352304ff683ba149e4246e80f
- Quelldatensatz
- uspto-grants-2005_08
- Patentnummer
- US06933265B2
Verknüpfte Notizen
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