Potassium Carbonate → HCID 67055245, Verbindung

HRID 601655

Reaktionsgleichung

Reaktionsgleichung von HRID 601655
[CH3:1][NH:2][CH:3]([CH3:5])[CH3:4].C(=O)([O-])[O-].[K+].[K+].CN(C)S(=O)=O.Cl[C:19]1[CH:28]=[CH:27][C:26]2[C:21](=[CH:22][CH:23]=[C:24]([Br:29])[CH:25]=2)[N:20]=1>O>[Br:29][C:24]1[CH:25]=[C:26]2[C:21](=[CH:22][CH:23]=1)[N:20]=[C:19]([N:2]([CH3:1])[CH:3]([CH3:5])[CH3:4])[CH:28]=[CH:27]2

Komponenten

6

Edukt 4

HCID 11430Potassium CarbonateHCID 78485N-MethylisopropylamineHCID 128940866-Bromo-2-chloroquinolineHCID 178486088HCID 178486088, Verbindung

Produkt 1

HCID 67055245HCID 67055245, VerbindungAusbeute 2,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

Under nitrogen atmosphere, 180 mg of N-methylisopropylamine, and 200 g of potassium carbonate were added at room temperature sequentially to 5 ml solution of dimethylsulfonamide with 63 g of 2-chloro-6-bromoquinoline, and the mixture was stirred at 110° C. for 4 hours. Water was added to the reaction solution, extracted with ethyl acetate. Ethyl acetate layer was washed with saturated saline solution, and dried with anhydrous sodium sulfate. The solvents were distilled outunder reduced pressure, and the residues were separated and purified by silicagel chromatography (hexane/ethyl acetate=3/1) to obtain 18 mg of the above compound as a white solid.

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washEthyl acetate layer was washed with saturated saline solution
  3. dry with materialdried with anhydrous sodium sulfate
  4. distillationThe solvents were distilled outunder reduced pressure
  5. customthe residues were separated
  6. custompurified by silicagel chromatography (hexane/ethyl acetate=3/1)

Quellen und Nachweise

ORD-Eintrag
ord-1c89321693754e3bb4331fa3b6b35c4c
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07902369B2

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