1,2-Dichloroethane → 1-(Piperidin-4-yl)-2-[2-(trifluoromethyl)phenyl)ethanone hydrochloride

HRID 890045Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 890045
C([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=[O:26])[CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[C:22]([F:25])([F:24])[F:23])[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:27]CCCl>ClC(OC(Cl)C)=O>[ClH:27].[NH:8]1[CH2:9][CH2:10][CH:11]([C:14](=[O:26])[CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[C:22]([F:24])([F:25])[F:23])[CH2:12][CH2:13]1

Komponenten

4

Edukt 2

HCID 111,2-DichloroethaneHCID 222479231-(1-Benzylpiperidin-4-yl)-2-[2-(trifluoromethyl)phenyl]ethanone

Produkt 1

HCID 222484771-(Piperidin-4-yl)-2-[2-(trifluoromethyl)phenyl)ethanone hydrochlorideAusbeute 83 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5213051-Chloroethyl chloroformateLösungsmittel

Versuchsvorschrift

After dissolving 1.30 g of 1-(1-benzylpiperidin-4-yl)-2-[2-(trifluoromethyl)phenyl]ethanone in 10 ml of 1,2-dichloroethane, 0.58 ml of 1-chloroethyl chloroformate was added while stirring at room temperature and the mixture was heated to reflux for 1 hour. The solvent was distilled off under reduced pressure, 10 ml of methanol was added to the residue and heating to reflux was continued for 30 minutes. The solvent was distilled off under reduced pressure, ethyl acetate/n-hexane was added to the residue and the precipitate was filtered out to obtain the title compound (916 mg, 83% yield).

Aufarbeitung

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 1 hour
  4. distillationThe solvent was distilled off under reduced pressure, 10 ml of methanol
  5. additionwas added to the residue
  6. temperatureheating
  7. temperatureto reflux
  8. distillationThe solvent was distilled off under reduced pressure, ethyl acetate/n-hexane
  9. additionwas added to the residue
  10. filtrationthe precipitate was filtered out

Quellen und Nachweise

ORD-Eintrag
ord-e4682d8e49a8413892ae5563f7888993
Quelldatensatz
uspto-grants-2006_02
Patentnummer
US06995144B2

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