Water → 4-[Ethyl(methyl)amino]benzaldehyde

HRID 1663604Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1663604
F[C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.[CH3:10][NH:11][CH2:12][CH3:13].C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[CH2:12]([N:11]([C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1)[CH3:10])[CH3:13]

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 12219N-MethylethylamineHCID 680234-Fluorobenzaldehyde

Produkt 1

HCID 133962824-[Ethyl(methyl)amino]benzaldehydeAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

To a solution of 4-fluorobenzaldehyde (1.5 g) and methylethylamine (1.56 mL) in dimethylsulfoxide (9 mL) was added potassium carbonate (2.17 g) and the mixture was stirred by using a microwave synthesizer (Biotage LTD.) at 120° C. for 2 hours. Thereto was added water and the mixture was extracted with ethyl acetate. The extract was dried over magnesium sulfate and concentrated in vacuo. The resultant crude product was purified by a column chromatography on silica gel (solvent; hexane/ethyl acetate=95:5→80:20) to give 4-(N-ethyl-N-methylamino)benzaldehyde (1.89 g, yield: 89%).

Aufarbeitung

  1. customat 120° C.
  2. customfor 2 hours
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe extract was dried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resultant crude product was purified by a column chromatography on silica gel (solvent; hexane/ethyl acetate=95:5→80:20)

Quellen und Nachweise

ORD-Eintrag
ord-5ed1b6e0df1f4b21b7ae5f6f131b099c
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08034949B2

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