1-Bromo-3-chloropropane → HCID 66961254, Verbindung

HRID 68999

Reaktionsgleichung

Reaktionsgleichung von HRID 68999
[C:1](=[O:4])([O-])[O-].[K+].[K+].[OH:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[N:14]=[C:13](OC)[CH:12]=[CH:11]2.[Cl:20][CH2:21][CH2:22][CH2:23]Br>C(#N)C.O>[Cl:20][CH2:21][CH2:22][CH2:23][O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[N:14]([CH3:13])[C:1](=[O:4])[CH:12]=[CH:11]2

Komponenten

6

Edukt 3

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 450911926-Hydroxy-2-methoxyquinoline

Produkt 1

HCID 66961254HCID 66961254, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

Potassium carbonate (0.829 g) was dissolved in acetonitrile (10 ml) and water (10 ml), and 6-hydroxy-2-methoxyquinoline (0.875 g) and 1-chloro-3-bromopropane (1.48 ml) was added thereto, and the mixture was stirred while heating under reflux for 4 hours. The reaction mixture was condensed under reduced pressure. Water was added to the residue, followed by extraction using ethyl acetate. The organic layer was dried with sodium sulfate, and was condensed under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1). The purified product was condensed to dryness under reduced pressure to give the title compound (1.107 g) as a white powder.

Aufarbeitung

  1. temperaturewhile heating
  2. temperatureunder reflux for 4 hours
  3. customcondensed under reduced pressure
  4. extractionfollowed by extraction
  5. dry with materialThe organic layer was dried with sodium sulfate
  6. customcondensed under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)
  8. customcondensed to dryness under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6af2b31558e94fa4a1dc4925a91fd34a
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822453B2

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