Reaktion #215050

Reaktionsgleichung

phorone

t-butyl hydroperoxide

sulfuric acid

→

2,6-DIMETHYL-2,6-bis(t-BUTYLPEROXY)-4-HEPTANONE

Lösungsmittel

pentane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONA mixture of 6.9 g
2. 2
   Temperaturto warm slowly to 25° C.
3. 3
   workup.STIRRINGstirred for 72 hours
4. 4
   WaschenAfter the reaction mixture was washed with water and sodium bisulfite solution, it
5. 5
   Trocknenwas dried over anhydrous magnesium sulfate
6. 6
   Sonstigethe drying agent separated
7. 7
   Sonstigethe pentane removed under reduced pressure
8. 8
   Sonstigea strong absorption in the 880 cm-1 region
9. 9
   Sonstigeno absorption in the regions

Vorschrift

A mixture of 6.9 g. (0.05 mole) of phorone and 23.2 g. (0.2 mole) of anhydrous 81% t-butyl hydroperoxide was diluted with 50 ml of pentane and the mixture stirred at 10° C., while 5.7 g. of 77% sulfuric acid solution was slowly added over a thirty minute time period. The mixture was then allowed to warm slowly to 25° C. and stirred for 72 hours. After the reaction mixture was washed with water and sodium bisulfite solution, it was dried over anhydrous magnesium sulfate, the drying agent separated and the pentane removed under reduced pressure. The product weighed 11.4 g. (71.7% of the calculated amount). The infrared spectrum showed a strong absorption in the 880 cm-1 region, usually associated with t-butylperoxy groups and no absorption in the regions ascribed to hydroxyl or olefin. A GLC scan showed one large major peak for the expected product. By active oxygen assay, the purity of the product was estimated at 93%.

Quelle