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Potassium Hydroxide → 3,4,4-Trimethoxypiperidine

HRID 846752
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 846752
[CH3:1][O:2][CH:3]1[C:8]([O:11][CH3:12])([O:9][CH3:10])[CH2:7][CH2:6][N:5](C(OCC)=O)[CH2:4]1.[OH-].[K+]>CC(O)C>[CH3:1][O:2][CH:3]1[C:8]([O:11][CH3:12])([O:9][CH3:10])[CH2:7][CH2:6][NH:5][CH2:4]1
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Komponenten

4

Edukt 2

HCID 14797Potassium HydroxideHCID 3019431Ethyl 3,4,4-trimethoxypiperidine-1-carboxylate

Produkt 1

HCID 198835163,4,4-TrimethoxypiperidineAusbeute 75,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

A mixture of 117.7 parts of ethyl 3,4,4-trimethoxy-1-piperidinecarboxylate, 267.3 parts of potassium hydroxide and 720 parts of 2-propanol was stirred and refluxed for 4 hours. The reaction mixture was evaporated. 900 Parts of water were added to the residue and the whole was stirred in a boiling water-bath. The last traces of 2-propanol were removed by evaporation on a Rotavapor. After cooling to 10° C., the product was extracted twice with 280 parts of 1,1'-oxybisethane. The extracts were dried, filtered and evaporated, yielding 62.9 parts (75.4%) of 3,4,4-trimethoxypiperidine as a residue (intermediate 65).

Aufarbeitung

  1. temperaturerefluxed for 4 hours
  2. customThe reaction mixture was evaporated
  3. addition900 Parts of water were added to the residue
  4. stirringthe whole was stirred in a boiling water-bath
  5. customThe last traces of 2-propanol were removed by evaporation on a Rotavapor
  6. extractionthe product was extracted twice with 280 parts of 1,1'-oxybisethane
  7. customThe extracts were dried
  8. filtrationfiltered
  9. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-b87189fe5d3c462c9e9ac6eec6e0beff
Quelldatensatz
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05137896

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