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

HRID 251853Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 251853
[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

Edukt 3

HCID 222AmmoniaHCID 24386Thionyl ChlorideHCID 27755542-Methyl-4-(trifluoromethoxy)benzoic acid

Produkt 1

HCID 27755492-Methyl-4-(trifluoromethoxy)benzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

795 mg (3.61 mmol) of 2-methyl-4-(trifluoromethoxy)benzoic acid are heated with 4 ml (54.8 mmol) of thionyl chloride and a drop of DMF for 30 min under reflux. After cooling the reaction mixture is added slowly 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 for 1 h at 60° C. The reaction mixture is left to cool, the solid is collected by filtration and dried under vacuum. Yield: 562 mg (71% of theory)

Aufarbeitung

  1. temperatureAfter cooling the reaction mixture
  2. filtrationThe resulting precipitate is collected by suction filtration
  3. waitThe reaction mixture is left
  4. temperatureto cool
  5. filtrationthe solid is collected by filtration
  6. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-c8e79eabcc134568a8b02a07271b2636
Quelldatensatz
uspto-grants-2011_01
Patentnummer
US07867992B2

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