Potassium Carbonate → HCID 58853204, Verbindung

HRID 2280876Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2280876
F[C:2](F)(F)[C:3]1[CH:8]=[CH:7][C:6]([CH:9]([NH2:13])[CH2:10][CH2:11][CH3:12])=[CH:5][CH:4]=1.[Cl:16][C:17]1[CH:22]=[N:21][CH:20]=[C:19](Cl)[N:18]=1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.C(OCC)(=O)C.O>[Cl:16][C:17]1[N:18]=[C:19]([NH:13][CH:9]([C:6]2[CH:7]=[CH:8][C:3]([CH3:2])=[CH:4][CH:5]=2)[CH2:10][CH2:11][CH3:12])[CH:20]=[N:21][CH:22]=1

Komponenten

7

Edukt 3

HCID 11430Potassium CarbonateHCID 785042,6-DichloropyrazineHCID 59339521HCID 59339521, Verbindung

Produkt 1

HCID 58853204HCID 58853204, VerbindungAusbeute 5,7 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a solution of 1-[4-(trifluoromethyl)phenyl]butan-1-amine (0.40 g, 1.9 mmol) and 2,6-dichloropyrazine (0.55 g, 3.7 mmol) in 1,4-dioxane (6 mL) was added anhydrous potassium carbonate (0.39 g, 2.8 mmol). The resulting mixture was heated at reflux for 18 h. After cooling to room temperature, the mixture was diluted with ethyl acetate and H2O. The organic phase was collected, dried and concentrated. The residue was purified by flash chromatography eluting with ethyl acetate-hexane (1:1) to give pure product (0.03 g, 5%).

Aufarbeitung

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 18 h
  3. customThe organic phase was collected
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by flash chromatography
  7. washeluting with ethyl acetate-hexane (1:1)

Quellen und Nachweise

ORD-Eintrag
ord-1f15f0a932a64a9caa52d8e11c824d3d
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09139560B2

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