Methanol → Methyl 4-(piperidin-4-yl)benzoate

HRID 478640Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 478640
[NH:1]1[CH2:6][CH2:5][CH:4]([C:7]2[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=2)[CH2:3][CH2:2]1.[CH3:16]O>>[CH3:16][O:12][C:11](=[O:13])[C:10]1[CH:14]=[CH:15][C:7]([CH:4]2[CH2:5][CH2:6][NH:1][CH2:2][CH2:3]2)=[CH:8][CH:9]=1

Komponenten

3

Edukt 2

HCID 887MethanolHCID 180024624-(Piperidin-4-yl)benzoic acid

Produkt 1

HCID 24904226Methyl 4-(piperidin-4-yl)benzoate

Versuchsvorschrift

4-Piperidin-4-yl-benzoic acid (47 mmol) is dissolved in methanol (300 ml) and 1 ml of concentrated sulfonic acid is added. The mixture is heated under reflux overnight. After evaporation of the solvent, the residue is dissolved in a mixture of water and sodium carbonate (to ensure basic conditions) and extracted three times with ethyl acetate. The combined extract is dried over sodium sulfate and evaporated. A brown powder with Rf=0.18 (CH2Cl2/MeOH=9:1) is obtained.

Aufarbeitung

  1. temperatureThe mixture is heated
  2. temperatureunder reflux overnight
  3. customAfter evaporation of the solvent
  4. dissolutionthe residue is dissolved in a mixture of water and sodium carbonate (to ensure basic conditions)
  5. extractionextracted three times with ethyl acetate
  6. extractionThe combined extract
  7. dry with materialis dried over sodium sulfate
  8. customevaporated
  9. customA brown powder with Rf=0.18 (CH2Cl2/MeOH=9:1) is obtained

Quellen und Nachweise

ORD-Eintrag
ord-10bb8a05683e45f7a5dd016b41686167
Quelldatensatz
uspto-grants-2003_11
Patentnummer
US06642239B2

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