Potassium Carbonate → HCID 67383896, Verbindung

HRID 408110

Reaktionsgleichung

Reaktionsgleichung von HRID 408110
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][C:10](=[O:12])[CH3:11])[CH3:2].C([O-])([O-])=O.[K+].[K+].Br[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[CH2:26][CH3:27]>[Cu]Br>[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[CH2:26][CH3:27])[C:10](=[O:12])[CH3:11])[CH3:2]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 160891-Bromo-2-ethylbenzeneHCID 36332O-Ethylacetanilide

Produkt 1

HCID 67383896HCID 67383896, VerbindungAusbeute 67 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24593copper(I) bromideKatalysator

Reaktionsbedingungen

Temperatur
200 °C

Versuchsvorschrift

The mixture of the N-(2-ethylphenyl)acetamide (7.35 g, 45.03 mmol), anhydrous K2CO3 (6.22 g, 45.03 mmol), copper(I) bromide (452.2 mg, 3.15 mmol) in 1-bromo-2-ethylbenzene was stirred and heated to 200° C. under argon for 48 h. After cooling the reaction mixture was poured into ice-H2O and extracted with ethyl acetate (2×500 mL), the combined organics were washed with brine, dried over anhydrous (K2CO3), filtered and concentrated to dryness. The crude product was purified using an ISCO machine using a ethyl acetate-hexane gradient to afford the product, N,N-bis(2-ethylphenyl)acetamide (8.1 g, 67%).

Aufarbeitung

  1. temperatureAfter cooling the reaction mixture
  2. extractionextracted with ethyl acetate (2×500 mL)
  3. washthe combined organics were washed with brine
  4. dry with materialdried over anhydrous (K2CO3)
  5. filtrationfiltered
  6. concentrationconcentrated to dryness
  7. customThe crude product was purified

Quellen und Nachweise

ORD-Eintrag
ord-c6783476024348b39cf8721dedd375c9
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08759336B2

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