Oxalic Acid → Methyl 2-methyl-4-oxo-1-piperidinecarboxylate

HRID 1729804Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1729804
[CH3:1][O:2][C:3]([N:5]1[CH2:10][CH2:9][C:8](=[O:11])[CH:7](C(OCC)=O)[CH:6]1[CH3:17])=[O:4].C(O)(=O)C(O)=O>O>[CH3:17][CH:6]1[CH2:7][C:8](=[O:11])[CH2:9][CH2:10][N:5]1[C:3]([O:2][CH3:1])=[O:4]

Komponenten

4

Edukt 2

HCID 971Oxalic AcidHCID 53702337HCID 53702337, Verbindung

Produkt 1

HCID 21500264Methyl 2-methyl-4-oxo-1-piperidinecarboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

76 parts of ethyl 1-(methoxycarbonyl)-2-methyl-4-oxo-3-piperidinecarboxylate are hydrolyzed with 600 parts of ethanedioic acid solution 14% in water and the whole is stirred and refluxed for 40 hours. The product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The residue is distilled, yielding methyl 2-methyl-4-oxo-1-piperidinecarboxylate; bp. 96°-99° C. at 0.2-9.3 mm. pressure.

Aufarbeitung

  1. temperaturerefluxed for 40 hours
  2. extractionThe product is extracted with trichloromethane
  3. customThe extract is dried
  4. filtrationfiltered
  5. customevaporated
  6. distillationThe residue is distilled

Quellen und Nachweise

ORD-Eintrag
ord-52e45dc9668f4bc68f1e0ff31f602e73
Quelldatensatz
uspto-grants-1976_11
Patentnummer
US03989707

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