Reaktionsgleichung
[O:1]=[C:2]([CH:4]=[C:5]([CH3:7])[CH3:6])[CH3:3].[C:8]12([O:18][OH:19])[CH2:16][CH:12]([C:13]1([CH3:15])[CH3:14])[CH2:11][CH2:10][CH:9]2[CH3:17].S(=O)(=O)(O)O>>[CH3:6][C:5]([O:19][O:18][C:8]12[CH2:16][CH:12]([C:13]1([CH3:14])[CH3:15])[CH2:11][CH2:10][CH:9]2[CH3:17])([CH2:4][C:2](=[O:1])[CH3:3])[CH3:7]Komponenten
Reaktionsbedingungen
- Temperatur
- 25 °C
Versuchsvorschrift
A mixture of 11.8 g. (0.12 mole) of mesityl oxide and 25.40 g. (0.15 mole) of pinanyl hydroperoxide was stirred at 0° C. while 2.0 g. of 77% sulfuric acid solution was slowly added. The reaction mixture was allowed to warm slowly to 25° C. and stirred for a total of 16 hours. The organic layer was taken up in 30 ml. of either and washed with water, 5% sodium hydroxide solution and again with water to pH 8. The mixture was then subjected to steam distillation in the presence of sodium bicarbonate solution at 20 torr for 2 hours to remove unreacted mesityl oxide and pinanyl hydroperoxide. The product was taken up in ether, dried over anhydrous magnesium sulfate and the ether removed under reduced pressure leaving 18.14 g. of product (56.9% yield).
Aufarbeitung
- additionA mixture of 11.8 g
- washof either and washed with water, 5% sodium hydroxide solution and again with water to pH 8
- distillationThe mixture was then subjected to steam distillation in the presence of sodium bicarbonate solution at 20 torr for 2 hours
- customto remove unreacted mesityl oxide and pinanyl hydroperoxide
- dry with materialdried over anhydrous magnesium sulfate
- customthe ether removed under reduced pressure
- customleaving 18.14 g
Quellen und Nachweise
- ORD-Eintrag
- ord-2126ecab6e164cf49e90e9c1b1b4c7ca
- Quelldatensatz
- uspto-grants-1981_09
- Patentnummer
- US04289914
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