Water → 1-Benzyl-3-methylpiperidin-4-ol

HRID 980873Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 980873
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11](=[O:14])[CH:10]([CH3:15])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>CCOCC>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([OH:14])[CH:10]([CH3:15])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 5609651-Benzyl-3-methyl-4-piperidoneHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 136114921-Benzyl-3-methylpiperidin-4-ol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

Subsequently, 3.13 g of the 1-benzyl-3-methyl-4-piperidone obtained above was dissolved in 6 ml of ether. The solution was added dropwise to a suspension of 0.44 g of lithium aluminum hydride in 25 ml of ether over 5 minutes while maintaining the temperature at 24°-27° C. Then, the mixture was stirred at 25° C. for 10 minutes, and, 5 ml of water was added thereto under ice-cooling. The mixture was extracted with 30 ml of ether four times. The ether layer was washed with water, dried over anhydrous sodium sulfate and concentrated to obtain 3.17 g of an oily matter of 1-benzyl-4-hydroxy-3-methylpiperidine.

Aufarbeitung

  1. temperaturewhile maintaining the temperature at 24°-27° C
  2. temperatureunder ice-cooling
  3. extractionThe mixture was extracted with 30 ml of ether four times
  4. washThe ether layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-d580ba0cf2e548029188e50f7859d8d9
Quelldatensatz
uspto-grants-1987_01
Patentnummer
US04639522

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