Reaktion #215049

Reaktionsgleichung

phorone

t-butyl hydroperoxide

→

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

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONA mixture of 47.0 g
2. 2
   SonstigeThe ion exchange resin was separated by filtration
3. 3
   workup.ADDITIONthe product diluted with pentane
4. 4
   WaschenThe pentane solution was washed with water, sodium bisulfite solution, 5% sodium hydroxide solution and water
5. 5
   TrocknenAfter drying over anhydrous magnesium sulfate
6. 6
   Sonstigethe pentane was removed under reduced pressure

Vorschrift

A mixture of 47.0 g. (0.34 mole) of phorone and 157 g (1.36 mole) of 78% t-butyl hydroperoxide was stirred with 34 g. of dry Amberlyst 15® sulfonic acid type ion exchange resin in a 500 ml flask equipped with a condenser and thermometer for forty-eight hours at 40° C. and one hour at 50° C. The ion exchange resin was separated by filtration and the product diluted with pentane. The pentane solution was washed with water, sodium bisulfite solution, 5% sodium hydroxide solution and water. After drying over anhydrous magnesium sulfate, the pentane was removed under reduced pressure. The recovered product weighed 74.2 g. (68.5% of the calculated amount). A GLC scan showed a large major peak for the expected product. In the infrared spectrum, small bands for hydroxyl and olefin were observed but the band in the 880 cm-1 region usually associated with t-butyl peroxy groups was strong. By active oxygen assay, the purity of the product was estimated at 83%.

Quelle