Thiophenol → HCID 19821224, Verbindung

HRID 1030204Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1030204
F[C:2]1[CH:33]=[CH:32][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([O:14][C:15]([O:23][C:24]3[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH3:31])[CH:25]=3)([F:22])[CH:16]([F:21])[C:17]([F:20])([F:19])[F:18])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[C:40]1([SH:46])[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1>CN(C)C=O>[C:40]1([S:46][C:2]2[CH:3]=[CH:4][C:5]([C:6]([C:8]3[CH:13]=[CH:12][C:11]([O:14][C:15]([O:23][C:24]4[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH3:31])[CH:25]=4)([F:22])[CH:16]([F:21])[C:17]([F:19])([F:20])[F:18])=[CH:10][CH:9]=3)=[O:7])=[CH:32][CH:33]=2)[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1

Komponenten

5

Edukt 3

HCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 19821204HCID 19821204, Verbindung

Produkt 1

HCID 19821224HCID 19821224, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

33 g 4-fluoro-4'-(1-(3-methoxyphenoxy)-1,2,3,3,3-pentafluoro-propoxy)benzophenone, 10 g potassium carbonate, 7.7 g thiophenol, and 100 ml dimethylformamide were stirred together for eight hours at 100° C., then allowed to cool to room temperature. After cooling, the solids were removed from the mixture by filtration, and the low boilers were removed by distillation at 200° C./0.5 mm Hg. The resulting product was distilled at 240°-300° C./0.5 mm Hg. NMR spectra and gas chromatography confirmed that the desired benzophenone was prepared.

Aufarbeitung

  1. temperatureAfter cooling
  2. customthe solids were removed from the mixture by filtration
  3. customthe low boilers were removed by distillation at 200° C./0.5 mm Hg
  4. distillationThe resulting product was distilled at 240°-300° C./0.5 mm Hg
  5. customwas prepared

Quellen und Nachweise

ORD-Eintrag
ord-5c7f59391f394b18943bc6c57db533ea
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05104559

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