Water → 1-[4-(Hydroxymethyl)piperidin-1-yl]ethan-1-one

HRID 1199038Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1199038
C(O[C:5](=[O:7])[CH3:6])(=O)C.[OH:8][CH2:9][N:10]1[CH2:15][CH2:14]C[CH2:12][CH2:11]1.O.[C:17](=O)([O-])[O-].[K+].[K+]>C(O)C>[C:9]([N:10]1[CH2:15][CH2:14][CH:6]([CH2:5][OH:7])[CH2:12][CH2:11]1)(=[O:8])[CH3:17]

Komponenten

6

Edukt 4

HCID 962WaterHCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 446909Piperidin-1-ylmethanol

Produkt 1

HCID 189349231-[4-(Hydroxymethyl)piperidin-1-yl]ethan-1-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

1-Acetyl-4-hydroxymethylpiperidine may be obtained in the following manner: acetic anhydride (20.5 cc) is added in the course of 15 minutes to a solution of hydroxymethylpiperidine (23.8 g) in ethanol (100 cc) at a temperature in the region of 10° C., and the mixture is stirred for 18 hours at a temperature in the region of 20° C. The reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa); the residue obtained is taken up with water (50 cc) and potassium carbonate (50 g), and the solution is extracted with methylene chloride (3×150 cc); the organic extracts are combined, dried and concentrated to dryness under reduced pressure (2.7 kPa). 1-Acetyl-4-hydroxymethylpiperidine (33.6 g) is thereby obtained in the form of an oil, which is employed in the crude state in the subsequent syntheses.

Aufarbeitung

  1. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa)
  2. customthe residue obtained
  3. extractionthe solution is extracted with methylene chloride (3×150 cc)
  4. customdried
  5. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)

Quellen und Nachweise

ORD-Eintrag
ord-d7b77a4f19934657aad1f55d5fca907b
Quelldatensatz
uspto-grants-1990_02
Patentnummer
US04898871

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