Bismuth-oxygen → HCID 22182039, Verbindung

HRID 53840Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 53840
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:19])[CH:9]([C:11]2[CH:16]=[CH:15][C:14]([S:17][CH3:18])=[CH:13][CH:12]=2)[OH:10])=[CH:4][CH:3]=1.[Bi]=O>C(O)(=O)C>[CH3:18][S:17][C:14]1[CH:15]=[CH:16][C:11]([C:9](=[O:10])[C:8]([C:5]2[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=2)=[O:19])=[CH:12][CH:13]=1

Komponenten

4

Edukt 2

HCID 6327914Bismuth-oxygenHCID 541534701-(4-Fluorophenyl)-2-hydroxy-2-[4-(methylsulfanyl)phenyl]ethan-1-one

Produkt 1

HCID 22182039HCID 22182039, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of ketone from step 2 (1.25 g, 4.5 mmol) and bismuth oxide (Bi2O3) (2.7 g, 1.2 equiv.) in acetic acid (20 ml) was warmed to 80° C. for 30 minutes. After cooling, the mixture was filtered through Celite® filter agent and the filtrate was concentrated. The residue was dissolved in hot methanol and filtered. The solvent was concentrated under a nitrogen stream, placed in the refrigerator and the precipitate formed was filtered to give 1 g (83%) of titled dione: m.p. 96°-97° C. Anal. Calc'd. for C15H11FO2S (M.W. 274.31): C, 65.68; H, 4.04; S, 11.69. Found: C, 65.42; H, 3.85; S, 1.42.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationthe mixture was filtered through Celite®
  3. filtrationfilter agent
  4. concentrationthe filtrate was concentrated
  5. dissolutionThe residue was dissolved in hot methanol
  6. filtrationfiltered
  7. concentrationThe solvent was concentrated under a nitrogen stream
  8. customthe precipitate formed
  9. filtrationwas filtered
  10. customto give 1 g (83%) of titled dione

Quellen und Nachweise

ORD-Eintrag
ord-5c4ae554404c4ce19da1ed240b0b6b9f
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05620999

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