StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Pyridine → 4-(4-Fluorophenyl)-3-[(3,4-methylenedioxyphenyl)oxycarbonyl]-piperidine-6-one

HRID 2296769
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2296769
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][C:12](=[O:14])[NH:11][CH2:10][CH:9]2[CH2:15]CC(O)=O)=[CH:4][CH:3]=1.[OH-:20].[Na+].S(Cl)(Cl)=O.S(=O)=O.N1C=CC=CC=1.[CH2:35]1[O:39][C:38]2[CH:40]=[C:41]([OH:44])[CH:42]=[CH:43][C:37]=2[O:36]1>C(O)C.C(Cl)(Cl)Cl>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH2:13][C:12](=[O:14])[NH:11][CH2:10][CH:9]2[C:15]([O:44][C:41]2[CH:42]=[CH:43][C:37]3[O:36][CH2:35][O:39][C:38]=3[CH:40]=2)=[O:20])=[CH:6][CH:7]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 6

HCID 1049PyridineHCID 1119Sulfur DioxideHCID 14798Sodium HydroxideHCID 24386Thionyl ChlorideHCID 68289SesamolHCID 227338414-(4-Fluorophenyl)-3-carboxyethylpiperidin-6-one

Produkt 1

HCID 22733847
4-(4-Fluorophenyl)-3-[(3,4-methylenedioxyphenyl)oxycarbonyl]-piperidine-6-one
Ausbeute 51,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittel2×HCID 6212ChloroformLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A solution of 4-(4-fluorophenyl)-3-carboxyethylpiperidin-6-one (0.5 g, 1.88 mmol, trans/cis ratio 56:44) in ethanol (10 ml) was added to a solution of sodium hydroxide (0.08 g, 2 mmol) in 95% ethanol (5 ml) and the mixture heated for 4 hours at 60° C. The solvent was removed at reduced pressure and the residue of water removed by distillation with toluene. The residue was suspended in dichloromethane (5 ml), treated with a solution of thionyl chloride (0.24 g, 2 mmol), and the mixture was brought to reflux. After 1 hour evolution of sulphur dioxide ceased, so the mixture was cooled to room temperature and treated with pyridine (0.16 g, 2 mmol) followed by a solution of sesamol (0.24 g, 1.75 mmol) in chloroform (2.5 ml). The resulting mixture was brought to reflux, heated for 4 hours, and stirred at ambient temperature for 2 days. The solvent was then removed at reduced pressure and the residue treated with water (5 ml), then extracted with ethyl acetate (20 and 10 ml). The organic extracts were combined, washed with brine (20 ml), dried over anhydrous sodium sulphate, filtered and evaporated to give the title compound (0.32 g).

Aufarbeitung

  1. customThe solvent was removed at reduced pressure
  2. customthe residue of water removed by distillation with toluene
  3. temperatureto reflux
  4. temperaturewas cooled to room temperature
  5. temperatureto reflux
  6. temperatureheated for 4 hours
  7. customThe solvent was then removed at reduced pressure
  8. additionthe residue treated with water (5 ml)
  9. extractionextracted with ethyl acetate (20 and 10 ml)
  10. washwashed with brine (20 ml)
  11. dry with materialdried over anhydrous sodium sulphate
  12. filtrationfiltered
  13. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-df002cd9bb3f4fbfa3e6d24fdf45cf93
Quelldatensatz
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06489347B1

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion