Methanol → HCID 178440154, Verbindung

HRID 1249552Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1249552
[CH3:1][CH:2]([C:4]1[N:5]=[C:6]([C:17]([C:23]([F:26])([F:25])[F:24])([C:19]([F:22])([F:21])[F:20])[OH:18])[NH:7][C:8]=1[C:9]1[CH:14]=[CH:13][C:12](SC)=[CH:11][CH:10]=1)[CH3:3].O[O:28][S:29]([O-:31])=O.[K+].S(OOS([O-])(=O)=O)(O)(=O)=O.[K+].[CH3:44]O>>[CH3:1][CH:2]([C:4]1[N:5]=[C:6]([C:17]([C:23]([F:26])([F:24])[F:25])([C:19]([F:20])([F:21])[F:22])[OH:18])[NH:7][C:8]=1[C:9]1[CH:10]=[CH:11][C:12]([S:29]([CH3:44])(=[O:31])=[O:28])=[CH:13][CH:14]=1)[CH3:3]

Komponenten

5

Edukt 4

HCID 887MethanolHCID 23690007Potassium hydrogen persulfateHCID 23707502Potassium hydroxy sulfiteHCID 178503127HCID 178503127, Verbindung

Produkt 1

HCID 178440154HCID 178440154, Verbindung

Versuchsvorschrift

A mixture of 4.0 g (0.01 mole) of 4-(1-methylethyl)-5-(4-methylthiophenyl)-α,α-bis(trifluoromethyl)-1H-imidazole-2-methanol, 16.06 g (0.026 mole) of Oxone® (potassium hydrogen persulfate) and 115 ml of methanol was stirred at room temperature overnight. The inorganic solid was filtered off, and the filtrate was evaporated. The residue was partitioned between ethyl acetate and water. The layers were separated and the organic layer was washed with water, brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The product was recrystallized from dichloroethane affording 3.33 g (77%) of the title compound as a white solid, m.p. 182°-184° C.

Aufarbeitung

  1. filtrationThe inorganic solid was filtered off
  2. customthe filtrate was evaporated
  3. customThe residue was partitioned between ethyl acetate and water
  4. customThe layers were separated
  5. washthe organic layer was washed with water, brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated in vacuo
  8. customThe product was recrystallized from dichloroethane affording 3.33 g (77%) of the title compound as a white solid, m.p. 182°-184° C.

Quellen und Nachweise

ORD-Eintrag
ord-b1c6dbbda2a349a497553983989702f1
Quelldatensatz
uspto-grants-1986_12
Patentnummer
US04632930

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