Sulfuric Acid → p-Hydroxystyrene p-tetrahydropyranyloxystyrene

HRID 2674

Reaktionsgleichung

Reaktionsgleichung von HRID 2674
[CH:1]#[C:2][C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.[O:10]1[CH:15]=[CH:14][CH2:13][CH2:12][CH2:11]1.S(=O)(=O)(O)O.C(=O)([O-])[O-].[Na+].[Na+]>C(COC)OC.O>[O:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH:11]1[O:9][C:6]1[CH:7]=[CH:8][C:3]([CH:2]=[CH2:1])=[CH:4][CH:5]=1.[OH:9][C:6]1[CH:7]=[CH:8][C:3]([CH:2]=[CH2:1])=[CH:4][CH:5]=1

Komponenten

7

Edukt 4

HCID 1118Sulfuric AcidHCID 80803,4-dihydro-2H-pyranHCID 10340Sodium CarbonateHCID 327584-Ethynylphenol

Produkt 1

HCID 67686066p-Hydroxystyrene p-tetrahydropyranyloxystyrene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 80711,2-DimethoxyethaneLösungsmittel

Versuchsvorschrift

Poly(p-hydroxystyrene) (weight average molecular weight: 9,600) in an amount of 9 g was dissolved in 100 ml of dimethoxyethane, and thereto 12.6 g of 3,4-dihydro-2H-pyran and 0.5 ml of sulfuric acid were added. This solution was stirred for 15 hours at 30°-40° C. After the reaction was completed, the reaction solution was concentrated under reduced pressure. The residue obtained was neutralized with sodium carbonate, and then poured into water to precipitate crystals. The crystals were filtered off, washed with water and dried under reduced pressure. Thus, 11.0 g of poly(p-tetrahydropyranyloxystyrene-p-hydroxystyrene) was obtained as white powder. The ratio of the p-tetrahydropyranyloxystyrene units to the p-hydroxystyrene units in the polymer obtained was determined to be 3:7 by 1H-NMR analysis.

Aufarbeitung

  1. concentrationthe reaction solution was concentrated under reduced pressure
  2. customThe residue obtained
  3. customto precipitate crystals
  4. filtrationThe crystals were filtered off
  5. washwashed with water
  6. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-5a412429988a4f6d803dc50ce52e1efd
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05731123

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