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1-(1-Acetoxyethyl)-3,5-diacetoxy-benzene → 3,5-Diacetoxy Styrene

HRID 1163268
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1163268
C(O[CH:5]([C:7]1[CH:12]=[C:11]([O:13][C:14](=[O:16])[CH3:15])[CH:10]=[C:9]([O:17][C:18](=[O:20])[CH3:19])[CH:8]=1)[CH3:6])(=O)C>C1(C)C=CC=CC=1>[C:14]([O:13][C:11]1[CH:12]=[C:7]([CH:8]=[C:9]([O:17][C:18](=[O:20])[CH3:19])[CH:10]=1)[CH:5]=[CH2:6])(=[O:16])[CH3:15]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 117375661-(1-Acetoxyethyl)-3,5-diacetoxy-benzene

Produkt 1

HCID 113105593,5-Diacetoxy StyreneAusbeute 42,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
500 °C

Versuchsvorschrift

20 g of 1-(1-acetoxyethyl)-3,5-diacetoxy-benzene (71 mmol) were dissolved in 20 ml toluene and placed into a feed vessel connected to a pyrolytic tube filled with Raschig rings. The tube was heated to 500° C. and the neat mixture was immediately added. Conversion of the alcohol was achieved within two minutes. The column was rinsed with toluene. Work-up was conducted by extracting the crude material in toluene twice with 200 ml water. The aqueous solutions were reextracted with toluene, the organic layers were combined, dried over magnesium sulfate and the solvent removed under reduced pressure giving 6.6 g 3,5-diacetoxystyrene (42%).

Aufarbeitung

  1. customplaced into a feed vessel
  2. customconnected to a pyrolytic tube
  3. additionfilled with Raschig rings
  4. additionthe neat mixture was immediately added
  5. washThe column was rinsed with toluene
  6. extractionby extracting the crude material in toluene twice with 200 ml water
  7. dry with materialdried over magnesium sulfate
  8. customthe solvent removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-4384818e26ee41f096313884190b9ad7
Quelldatensatz
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07820848B2

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