Ammonia → 2-Methyl-4-(trifluoromethoxy)benzamide

HRID 2099309Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2099309
[CH3:1][C:2]1[CH:10]=[C:9]([O:11][C:12]([F:15])([F:14])[F:13])[CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].S(Cl)(Cl)=O.[NH3:20]>CN(C=O)C>[CH3:1][C:2]1[CH:10]=[C:9]([O:11][C:12]([F:15])([F:14])[F:13])[CH:8]=[CH:7][C:3]=1[C:4]([NH2:20])=[O:5]

Komponenten

5

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

795 mg (3.61 mmol) of 2-methyl-4-(trifluoromethoxy)benzoic acid are heated under reflux with 4 ml (54.8 mmol) of thionyl chloride and one drop of DMF for 30 minutes. After cooling, the reaction solution is slowly added dropwise into an ice-cooled concentrated aqueous ammonia solution. The resulting precipitate is collected by suction filtration, taken up in 30 ml of water and stirred at 60° C. for 1 h. The mixture is allowed to cool and the solid is collected by filtration and dried in vacuo. Yield: 562 mg (71% of theory).

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationThe resulting precipitate is collected by suction filtration
  3. temperatureto cool
  4. filtrationthe solid is collected by filtration
  5. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-43dde2d096924d03a58437ed6acd3ef0
Quelldatensatz
uspto-grants-2009_08
Patentnummer
US07569563B2

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