Reaktion #2555

ord-0679f3c83e8041a093c3b3901f299d06

Reaktionsgleichung

Cl.O=C(c1ccc(F)cc1)C1CCN(CCCl)CC1
1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride
O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
O=C(c1ccc(F)cc1)C1CCN(CCCl)CC1
title compound
Ausbeute 92.3%
O=C(c1ccc(F)cc1)C1CCN(CCCl)CC1
1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine
Ausbeute 92.3%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturWith cooling in an ice bath
  2. 2
    ExtraktionThe reaction solution was extracted with ether
  3. 3
    Waschenwashed with saturated brine
  4. 4
    Trocknenthe resulting organic layer was dried on anhydrous sodium carbonate
  5. 5
    FiltrationThereafter, the organic layer was filtered through silica gel (5 g)
  6. 6
    Sonstigethe solvent was removed by evaporation
  7. 7
    Sonstigethe resulting residue was purified

Vorschrift

1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride (800 mg, 2.61 mmol) was suspended in ether (20 ml). With cooling in an ice bath, saturated sodium carbonate aqueous solution (5 ml) was added dropwise to the suspension. The reaction solution was extracted with ether and washed with saturated brine, and the resulting organic layer was dried on anhydrous sodium carbonate. Thereafter, the organic layer was filtered through silica gel (5 g), the solvent was removed by evaporation and then the resulting residue was purified by subjecting it to a silica gel column chromatography (ether) to obtain 650 mg (92.3%) of the title compound in the form of light yellow solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05728835uspto-grants-1998_03