Hydrochloric Acid → Ethyl 4-methylpiperidine-3-carboxylate

HRID 931301

Reaktionsgleichung

Reaktionsgleichung von HRID 931301
Cl.[CH3:2][CH:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH:4]1[C:9]([OH:11])=[O:10].[CH2:12](O)[CH3:13]>C(O)(=O)C>[CH3:2][CH:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH:4]1[C:9]([O:11][CH2:12][CH3:13])=[O:10]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 136586094-Methylpiperidine-3-carboxylic acid

Produkt 1

HCID 13658603Ethyl 4-methylpiperidine-3-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

Hydrogen chloride gas was bubbled into a solution of 4-methylpiperidine-3-carboxylic acid (6.0 g, 41.90 mmol) in ethanol (150 mL) and acetic acid (30 mL) at 0° C. under a nitrogen atmosphere. The reaction mixture was heated at reflux for 48 h, then was cooled and was partitioned between water and ethyl acetate. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to afford ethyl 4-methylpiperidine-3-carboxylate (5.0 g). The material was used without further purification.

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 48 h
  3. temperaturewas cooled
  4. customwas partitioned between water and ethyl acetate
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-915fa440dfb3481ebc20e592cac4db4c
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09296745B2

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