Potassium Carbonate → HCID 86666210, Verbindung

HRID 474667Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 474667
[F:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[C:4]([OH:9])[CH:3]=1.F[C:11]1[CH:18]=[CH:17][C:14]([CH:15]=[O:16])=[CH:13][CH:12]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O>[F:1][C:2]1[CH:3]=[C:4]([O:9][C:11]2[CH:18]=[CH:17][C:14]([CH:15]=[O:16])=[CH:13][CH:12]=2)[CH:5]=[CH:6][C:7]=1[CH3:8]

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 27746133-Fluoro-4-methylphenol

Produkt 1

HCID 86666210HCID 86666210, VerbindungAusbeute 60,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

To a solution of 3-fluoro-p-cresol (2.5 g, 19.82 mmol) and 4-fluorobenzaldehyde (2.460 g, 19.82 mmol) in DMF (15 mL), was added K2CO3 (4.11 g, 29.7 mmol). The mixture was heated with a microwave condition at 130° C. for 1 h. After cooling, the reaction mixture was diluted in water, extracted with EA. The organic phase was washed with water and brine, dried over Na2SO4, concentrated and purified via flash chromatography to afford the title compound (2.741 g, 11.91 mmol, 60.1% yield) as a yellow oil. LCMS: rt=3.57 min, [M+H+]=231

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionextracted with EA
  3. washThe organic phase was washed with water and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. custompurified via flash chromatography

Quellen und Nachweise

ORD-Eintrag
ord-5deb8cf538674a40b70337bff58ec0ec
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08637536B2

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