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.[O:18]1[CH2:22][CH2:21][CH2:20][CH2:19]1>>[CH:19]([O:18][C:7]([CH3:8])([CH3:12])[CH3:17])=[CH2:20].[CH2:22]([OH:18])[CH2:21][C:20]1[CH:5]=[CH:4][CH:3]=[CH:2][CH:19]=1Komponenten
Versuchsvorschrift
A mixture of 100 ml of tetrahydrofuran (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 mixture 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-19635a9c8c7d44c4bf24a08554a85278
- Quelldatensatz
- uspto-grants-2001_10
- Patentnummer
- US06309793B1
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