Hydrochloric Acid → 2-Methyl-2-(1-methylpiperidin-3-yl)propanoic acid

HRID 499708Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 499708
C[O:2][C:3](=[O:14])[C:4]([CH3:13])([CH:6]1[CH2:11][CH2:10][CH2:9][N:8]([CH3:12])[CH2:7]1)[CH3:5].[OH-].[Li+].Cl>CO>[CH3:13][C:4]([CH:6]1[CH2:11][CH2:10][CH2:9][N:8]([CH3:12])[CH2:7]1)([CH3:5])[C:3]([OH:14])=[O:2]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 668891612-Methyl-2-(1-methyl-piperidin-3(r,s)-yl)-propionic acid methyl ester

Produkt 1

HCID 668879152-Methyl-2-(1-methylpiperidin-3-yl)propanoic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

0.200 g of 2-methyl-2-(1-methyl-piperidin-3(R,S)-yl)-propionic acid methyl ester are dissolved in 4 ml of methanol. 4 ml of a 1M aqueous lithium hydroxide solution are added and the mixture is stirred for 16 hours at room temperature. The reaction mixture is neutralised with 1M HCl and extracted with ethyl acetate (3×50 ml). The organic phases are combined and concentrated by evaporation. The residue is purified by means of flash chromatography (SiO2 60 F) to provide the title compound as a colourless oil. Rf 0.15 (150:54:10:1 dichloromethane-methanol-acetic acid-water).

Aufarbeitung

  1. extractionextracted with ethyl acetate (3×50 ml)
  2. concentrationconcentrated by evaporation
  3. customThe residue is purified by means of flash chromatography (SiO2 60 F)

Quellen und Nachweise

ORD-Eintrag
ord-240c917ab8bb4b0e980ff73e278c96b2
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07767690B2

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