반응 #216550

반응 방정식

poly(p-hydroxystyrene)

3,4-dihydro-2H-pyran

sulfuric acid

→

title compound

수율 93.6%

p-tetrahydropyranylstyrene p-hydroxystyrene

수율 93.6%

용매

dimethoxyethane

반응 조건

후처리

1. 1
   기타followed by reaction at 30°-40° C. for 15 hours
2. 2
   기타After reaction
3. 3
   기타the mixture was evaporated in vacuo
4. 4
   workup.ADDITIONthe residue was neutralized by addition of sodium carbonate
5. 5
   workup.ADDITIONpoured into H2O (1 liter)
6. 6
   여과The precipitate was filtered by suction
7. 7
   세척washed with H2O
8. 8
   기타dried under reduced pressure

실험 절차

To a solution of poly(p-hydroxystyrene) (9.0 g) [MARUKA LYNCUR-M, manufactured by Maruzen Petrochemical Co., Ltd., Mw 10000 and Mn 5000] in dimethoxyethane (100 ml), 3,4-dihydro-2H-pyran (12.6 g) and conc. sulfuric acid (0.5 ml) were added, followed by reaction at 30°-40° C. for 15 hours with stirring. After reaction, the mixture was evaporated in vacuo, the residue was neutralized by addition of sodium carbonate and poured into H2O (1 liter). The precipitate was filtered by suction, washed with H2O and dried under reduced pressure to give 11.0 g of the title compound as a white powder having Mw 10000 (GPC with polystyrene calibration). The composition of the polymer was found to be p-tetrahydropyranyloxystyrene unit and p-hydroxystyrene unit in a molar ratio of ca. 3:7 based on 1HNMR.

출처