Reaktionsgleichung
[NH+]1C=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:7]1([CH3:17])[CH:12]=CC(S([O-])(=O)=O)=C[CH:8]=1.[CH2:18]1[CH2:22][O:21][CH2:20][CH2:19]1>>[CH:20]([O:21][C:7]([CH3:8])([CH3:12])[CH3:17])=[CH2:19].[CH2:22]([OH:21])[CH2:18][C:19]1[CH:5]=[CH:4][CH:3]=[CH:2][CH:20]=1Komponenten
Versuchsvorschrift
A mixture of 100 ml of tetrahydrofiran (THF) and 30 g of powdered polyhydroxystyrene (PHS) was added to a 250 ml three-necked flask equipped with a temperature probe, an overhead mechanical stirrer and a nitrogen inlet. The mixture stirred for 30 minutes to form a homogeneous solution before 5.0 g of tertiary butyl vinyl ether, 4.8 g of phenethyl alcohol and 140 mg of solid pyridinium-para-toluene sulfonate was added. A brief exotherm was observed followed by a temperature rise of 23° to 27° C. The solution was allowed to stir at 23° C. for 20 hours before 4 g of triethylamine solution (prepared by dissolving 2.31 g of triethylamine in 200 g of THF) was added to the reaction mixture to quench the acid. The reaction mite was stirred for additional 30 minutes. The polymer solution was drop-wise added to 1000 ml of de-ionized water under vigorous stirring. The precipitated solid polymer was isolated by filtration. The polymer was washed two times with 250 ml of de-ionized water. The polymer was dried under vacuum at 60° C. for 18 hours.
Aufarbeitung
- additionwas added to a 250 ml three-necked flask
- customequipped with a temperature probe, an overhead mechanical stirrer and a nitrogen inlet
Quellen und Nachweise
- ORD-Eintrag
- ord-1fed4be4b0bf4a00811fa3894ceb4b41
- Quelldatensatz
- uspto-grants-2002_04
- Patentnummer
- US06380317B1
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