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Sulfuric Acid → 4-Ethynylphenol

HRID 2676
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2676
C([O:5][C:6]1[CH:13]=[CH:12][C:9]([CH:10]=[CH2:11])=[CH:8][CH:7]=1)(C)(C)C.N(C(C)(C)C#N)=NC(C)(C)C#N.S(=O)(=O)(O)O.C(OCC)(=O)C>COCC(O)C>[CH:11]#[C:10][C:9]1[CH:12]=[CH:13][C:6]([OH:5])=[CH:7][CH:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 1118Sulfuric AcidHCID 6547AzobisisobutyronitrileHCID 8857Ethyl AcetateHCID 5775311-(Tert-butoxy)-4-ethenylbenzene

Produkt 1

HCID 327584-Ethynylphenol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 79001-Methoxy-2-propanolLösungsmittel

Versuchsvorschrift

In 80 g of propylene glycol monomethyl ether was dissolved 88 g of p-t-butoxystyrene, and then, 2 g of azobisisobutyronitrile was added to the solution, after which they were subjected to polymerization for 10 hours under a nitrogen atmosphere while the reaction temperature was kept at 80° C. After the polymerization, an aqueous sulfuric acid solution was added to the reaction mixture and the resulting mixture was subjected to hydrolysis at 80° C. for 8 hours. Subsequently, ethyl acetate was added to the reaction mixture and the resulting mixture was washed with water, after which the solvent was replaced by acetone. The resulting resin solution was dropped into a large amount of water to coagulate a resin. The resin was recovered and dried in a vacuum drier kept at 50° C. overnight to obtain 48 g of a white fine powder of poly(p-hydroxystyrene).

Aufarbeitung

  1. customafter which they were subjected to polymerization for 10 hours under a nitrogen atmosphere while the reaction temperature
  2. customwas kept at 80° C
  3. customAfter the polymerization
  4. customthe resulting mixture was subjected to hydrolysis at 80° C. for 8 hours
  5. washthe resulting mixture was washed with water
  6. additionThe resulting resin solution was dropped into a large amount of water
  7. customThe resin was recovered
  8. customdried in a vacuum drier

Quellen und Nachweise

ORD-Eintrag
ord-a955b85440dc450e8071495d57560dc1
Quelldatensatz
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05731125

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