Piperidine → p-Piperidinophenol

HRID 2354033Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2354033
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:7]1(=O)[CH2:12][CH2:11][C:10](=[O:13])[CH2:9][CH2:8]1>C(O)C.[C].[Pd]>[OH:13][C:10]1[CH:11]=[CH:12][C:7]([N:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)=[CH:8][CH:9]=1

Komponenten

5

Edukt 2

HCID 8082PiperidineHCID 125111,4-Cyclohexanedione

Produkt 1

HCID 90452p-PiperidinophenolAusbeute 43,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

0.85 g of piperidine, 1.68 g of 1,4-cyclohexanedione and 40 mg of 10% palladium-carbon were heated with stirring in 40 ml of ethanol at 50° C. to 60° C. and reacted for 8 hours under air bubbling. During the reaction, ethanol was added as needed. After the completion of the reaction, the catalyst was removed by filtration and the filtrate was concentrated under reduced pressure. The resultant was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1) and purified by silica gel column chromatography again, and 0.668 g of 1-(4-hydroxyphenyl)piperidine was obtained (yield 43.4%).

Aufarbeitung

  1. customreacted for 8 hours under air
  2. custombubbling
  3. customDuring the reaction, ethanol
  4. additionwas added
  5. customAfter the completion of the reaction
  6. customthe catalyst was removed by filtration
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customThe resultant was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1)
  9. custompurified by silica gel column chromatography again

Quellen und Nachweise

ORD-Eintrag
ord-4d0f3a4a48f44ec1ad5e42423237ca77
Quelldatensatz
uspto-grants-2010_07
Patentnummer
US07750156B2

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