p-Toluenesulfonic acid → 4-{[3-Methoxy-5-(trifluoromethyl)phenyl]amino}-3-penten-2-one

HRID 1268887Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1268887
[C:1]([CH2:4][C:5](=O)[CH3:6])(=[O:3])[CH3:2].[CH3:8][O:9][C:10]1[CH:11]=[C:12]([CH:14]=[C:15]([C:17]([F:20])([F:19])[F:18])[CH:16]=1)[NH2:13].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[CH3:8][O:9][C:10]1[CH:11]=[C:12]([NH:13][C:5]([CH3:6])=[CH:4][C:1](=[O:3])[CH3:2])[CH:14]=[C:15]([C:17]([F:18])([F:20])[F:19])[CH:16]=1

Komponenten

5

Edukt 3

HCID 6101p-Toluenesulfonic acidHCID 31261AcetylacetoneHCID 6056715-(Trifluoromethyl)-m-anisidine

Produkt 1

HCID 694553434-{[3-Methoxy-5-(trifluoromethyl)phenyl]amino}-3-penten-2-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

1.57 g (15.7 mmol) Acetylacetone, 3.00 g (15.7 mmol) 3-methoxy-5-(trifluoromethyl)aniline, and 0.1 g (1.6 mmol) 4-toluenesulfonic acid are dissolved in 150 ml toluene. The reaction mixture is refluxed for 7 h with a Dean-Stark trap to remove water. After cooling down to room temperature, the suspension is filtered. The solid is purified by recrystallisation from ethanol.

Aufarbeitung

  1. temperatureThe reaction mixture is refluxed for 7 h with a Dean-Stark trap
  2. customto remove water
  3. filtrationthe suspension is filtered
  4. customThe solid is purified by recrystallisation from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-76713dd44a004bd3b44883728ad35591
Quelldatensatz
uspto-grants-2007_04
Patentnummer
US07199136B2

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