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

HRID 1011214Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1011214
[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 introduced 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 at 60° C. for 1 h. The mixture is allowed to cool and the solid is collected by filtration and dried under vacuum. 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 under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-bcb59cb9a5c145b7a058930215a7ef10
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07977349B2

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