Hydrochloric Acid → 1-(2-Chloropyridin-4-yl)piperidin-4-one

HRID 451539Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 451539
[Cl:1][C:2]1[CH:7]=[C:6]([N:8]2[CH2:17][CH2:16][C:11]3(OCC[O:12]3)[CH2:10][CH2:9]2)[CH:5]=[CH:4][N:3]=1.Cl.C(=O)([O-])O.[Na+]>CC(C)=O>[Cl:1][C:2]1[CH:7]=[C:6]([N:8]2[CH2:17][CH2:16][C:11](=[O:12])[CH2:10][CH2:9]2)[CH:5]=[CH:4][N:3]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 866567218-(2-Chloropyridin-4-yl)-1,4-dioxa-8-azaspiro[4.5]decane

Produkt 1

HCID 866567191-(2-Chloropyridin-4-yl)piperidin-4-oneAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a solution of 8-(2-chloropyridin-4-yl)-1,4-dioxa-8-azaspiro[4.5]decane (1.26 g, 4.95 mmol) in acetone (11 mL) was added HCl (2 N, 39.6 mL, 79.1 mmol) and the resulting mixture stirred at 50° C. for 2 hours, then cooled to room temperature. The pH was set to ˜8 by adding solid sodium hydrogen carbonate and then extracted with dichloromethane. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and evaporated to give the title product (1.03 g, 99%) as a white solid.

Aufarbeitung

  1. temperaturecooled to room temperature
  2. extractionextracted with dichloromethane
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-f5426199c702457d8b62a4211a4e58cc
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08486967B2

Notizen zur Reaktion

Wird geladen…