1,2-Dichloroethane → 2-(2-Fluorophenyl)-1-(piperidin-4-yl)ethanone hydrochloride

HRID 606161

Reaktionsgleichung

Reaktionsgleichung von HRID 606161
C([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=[O:23])[CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[F:22])[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:24]CCCl>ClC(OC(Cl)C)=O>[ClH:24].[F:22][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[CH2:15][C:14]([CH:11]1[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1)=[O:23]

Komponenten

4

Edukt 2

HCID 111,2-DichloroethaneHCID 222479931-(1-Benzylpiperidin-4-yl)-2-(2-fluorophenyl)ethanone

Produkt 1

HCID 222481242-(2-Fluorophenyl)-1-(piperidin-4-yl)ethanone hydrochlorideAusbeute 92 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5213051-Chloroethyl chloroformateLösungsmittel

Versuchsvorschrift

After dissolving 1.27 g of 1-(1-benzylpiperidin-4-yl)-2-(2-fluorophenyl)ethanone in 8 ml of 1,2-dichloroethane, 0.53 ml of 1-chloroethyl chloroformate was added while stirring on ice, and the mixture was heated to reflux for 1 hour. The solvent was distilled off under reduced pressure, 8 ml of methanol was added to the residue, and heating to reflux was continued for 40 minutes. The solvent was distilled off under reduced pressure, ethyl acetate was added to the residue, and the precipitate was filtered out to obtain the title compound (970 mg, 92% 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, 8 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
  9. additionwas added to the residue
  10. filtrationthe precipitate was filtered out

Quellen und Nachweise

ORD-Eintrag
ord-a3ce9cd537d04253bc7cdc2729cab5d7
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07915274B2

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