Acetic Anhydride → 2,4-Dimethyl-6-(2-phenylacryloyl)phenol

HRID 330234

Reaktionsgleichung

Reaktionsgleichung von HRID 330234
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([OH:9])=[C:4]([C:10](=[O:18])[CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:3]=1.[C:19](OC(=O)C)(=O)C>CN(CN(C)C)C>[CH3:8][C:6]1[CH:7]=[C:2]([CH3:1])[CH:3]=[C:4]([C:10](=[O:18])[C:11]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH2:19])[C:5]=1[OH:9]

Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 140259831-(2-Hydroxy-3,5-dimethylphenyl)-2-phenylethan-1-one

Produkt 1

HCID 148734432,4-Dimethyl-6-(2-phenylacryloyl)phenol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5829N,N,N',N'-TetramethylmethanediamineLösungsmittel

Versuchsvorschrift

212.6 Grams of 4,6-dimethyl-2-(2-phenylacetyl)phenol was dissolved in 350 ml of N,N,N',N'-tetramethyldiaminomethane, then under ice-cooled condition with stirring, 350 ml of acetic anhydride was added dropwise thereto. The reaction mixture was further stirred at room temperature for 2 hours, then was poured in 1 kg of ice and stirred vigorously. The crystals separated in the mixture were collected by filtration, washes with water, then dried. Recrystallized from ethanol to obtain 186 g of 2,4-dimethyl-6-(2-phenylacryloyl)phenol. Colorless needle-like crystals. Melting point: 83°-84° C.

Aufarbeitung

  1. temperatureunder ice-cooled condition
  2. stirringThe reaction mixture was further stirred at room temperature for 2 hours
  3. stirringstirred vigorously
  4. customThe crystals separated in the mixture
  5. filtrationwere collected by filtration, washes with water
  6. customdried
  7. customRecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-83b800954d984e1e9aa3774fe0c8f8bb
Quelldatensatz
uspto-grants-1990_01
Patentnummer
US04895847

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