Trifluoroacetic acid → HCID 178434688, Verbindung

HRID 350871

Reaktionsgleichung

Reaktionsgleichung von HRID 350871
[Cl:1][C:2]1[CH:3]=[C:4]([S:9][C:10]2[N:14](CC3C=CC(OC)=CC=3)[N:13]=[C:12]([CH3:24])[C:11]=2[C:25]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[O:26])[CH:5]=[C:6]([Cl:8])[CH:7]=1.FC(F)(F)C(O)=O>>[Cl:8][C:6]1[CH:5]=[C:4]([S:9][C:10]2[NH:14][N:13]=[C:12]([CH3:24])[C:11]=2[C:25]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[O:26])[CH:3]=[C:2]([Cl:1])[CH:7]=1

Komponenten

3

Edukt 2

HCID 6422Trifluoroacetic acidHCID 22747490[5-(3,5-dichlorophenylthio)-1-(4-methoxybenzyl)-3-methyl-1H-pyrazol-4-yl]-phenyl-methanone

Produkt 1

HCID 178434688HCID 178434688, VerbindungAusbeute 71,3 %

Versuchsvorschrift

140 mg of [5- (3,5-dichlorophenylthio)-1 -(4-methoxybenzyl)-3-methyl-1H-pyrazol-4-yl ]-phenyl-methanone was treated with 4 ml of trifluoroacetic acid. The solution was then heated at reflux for 2 h. The solvent was evaporated under reduced pressure. The residue was then partitioned between dichloromethane/saturated sodium hydrogen carbonate, washed with brine then dried over anhydrous magnesium sulphate, filtered and evaporated to give 75 mg of [5-(3,5-dichlorophenylthio)-3-methyl-1H-pyrazol-4-yl]-phenyl-methanone as a yellow solid which was used without further purification. Mass spectrum (ES) m/z 363[M+H]+.

Aufarbeitung

  1. temperatureThe solution was then heated
  2. temperatureat reflux for 2 h
  3. customThe solvent was evaporated under reduced pressure
  4. customThe residue was then partitioned between dichloromethane/saturated sodium hydrogen carbonate
  5. washwashed with brine
  6. dry with materialthen dried over anhydrous magnesium sulphate
  7. filtrationfiltered
  8. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-5073f99fc65a441ca2a2b98a304bfb52
Quelldatensatz
uspto-grants-2007_02
Patentnummer
US07183296B2

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