Potassium Iodide → HCID 13560729, Verbindung

HRID 414838Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 414838
Cl.Cl[CH2:3][C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=1.[C:14](=[O:17])([O-])[O-].[K+].[K+].[I-].[K+].[C:22](=[O:25])([O-])[O-].[Cs+].[Cs+]>CC(C)=O>[C:22]([C:7]1[CH:6]=[C:14]([CH:10]=[CH:9][CH:8]=1)[O:17][CH2:3][C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=1)(=[O:25])[CH2:11][CH2:12][CH2:13][CH2:4][CH3:3]

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 10796Cesium carbonateHCID 11430Potassium CarbonateHCID 30838232-(Chloromethyl)quinoline hydrochloride

Produkt 1

HCID 13560729HCID 13560729, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

This ketone (1.2 g) was refluxed with 2-chloromethylquinoline hydrochloride (1.3 g), potassium carbonate (8.6 g), potassium iodide (0.05 g) and cesium carbonate (0.05 g) in acetone (300 ml) for 24 hours. The reaction mixture was filtered, and the filtrate was concentrated, dissolved in chloroform, and then washed with sodium hydroxide solution (5%), water and brine. After drying this solution over MgSO4, all volatiles were removed. The residue was purified by chromatography on silica gel (25% ethyl acetate in hexanes). The pure desired product was isolated as a tan solid, m.p. 52°-55° C.

Aufarbeitung

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated
  3. dissolutiondissolved in chloroform
  4. washwashed with sodium hydroxide solution (5%), water and brine
  5. dry with materialAfter drying this solution over MgSO4
  6. customall volatiles were removed
  7. customThe residue was purified by chromatography on silica gel (25% ethyl acetate in hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-676dbe56a74944e5aa184ea58b8ab008
Quelldatensatz
uspto-grants-1988_12
Patentnummer
US04794188

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