Reaktion #354546

Reaktionsgleichung

10-undecenyl piperonyl ether

sodium dihydrogen phosphate monohydrate

→

crude product

11-epoxyundecenyl piperonyl ether

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTION(0.036 mole) of m-chloroperbenzoic and dissolved in 200 ml
2. 2
   Filtrationthe mixture was filtered
3. 3
   Waschenwashed with an aqueous sodium bicarbonate solution
4. 4
   TrocknenAfter drying the dichloromethane solvent
5. 5
   Sonstigewas removed by evaporation

Vorschrift

To a solution of 11.0 g. (0.036 mole) of 10-undecenyl piperonyl ether and 5.0 g. (0.036 mole) of sodium dihydrogen phosphate monohydrate in 100 ml. of dichloromethane, was added 7.6 g. (0.036 mole) of m-chloroperbenzoic and dissolved in 200 ml. of dichloromethane. After stirring at ambient temperature for 24 hours, the mixture was filtered and washed with an aqueous sodium bicarbonate solution. After drying the dichloromethane solvent was removed by evaporation. The crude product obtained in this way was purified by passing through a silica gel chromatographic column using first a 5% ether in hexane eluent and then a 50% ether in hexane eluent to recover the 10,11-epoxyundecenyl piperonyl ether which weighed 5 g. An infrared spectra had strong adsorption peaks at 3.4, 3.5, 6.7, 6.95, 7.9-8.0, 9.1, 9.6, 10.8 and 12.4 microns.

Quelle