Reaktion #216551

Reaktionsgleichung

poly(p-hydroxystyrene)

sulfuric acid

→

p-tert-butoxystyrene p-hydroxystyrene

Lösungsmittel

dimethoxyethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITwas continued at room temperature for 22 hours
3. 3
   SonstigeAfter reaction
4. 4
   Sonstigethe mixture was evaporated
5. 5
   workup.ADDITIONpoured into H2O
6. 6
   FiltrationThe precipitate was filtered by suction
7. 7
   Waschenwashed
8. 8
   Sonstigedried in vacuo

Vorschrift

To a solution of poly(p-hydroxystyrene) (4.0 g) [MARUKA LYNCUR-M, manufactured by Maruzen Petrochemical Co., Ltd., Mw 10000 and Mn 5000] in dimethoxyethane (70 ml) in a pressure vessel, isobutyrene (60 g) and conc. sulfuric acid (0.3 g) were added at -60° C. or lower. The mixture was brought to 45° C. for 1 hour with stirring, and then stirring was continued at room temperature for 22 hours. After reaction, the mixture was evaporated, and the residue was neutralized by sodium carbonate and poured into H2O. The precipitate was filtered by suction, washed was H2O and dried in vacuo to give 4.1 g of poly(p-tert-butoxystyrene/p-hydroxystyrene) as a white powder having Mw 10000 (GPC with polystyrene calibration). 1HNMR analysis indicated that 50% of p-hydroxy group was converted into p-tert-butoxy group.

Quelle