반응 #2555

ord-0679f3c83e8041a093c3b3901f299d06

반응 방정식

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
수율 92.3%
O=C(c1ccc(F)cc1)C1CCN(CCCl)CC1
1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine
수율 92.3%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도With cooling in an ice bath
  2. 2
    추출The reaction solution was extracted with ether
  3. 3
    세척washed with saturated brine
  4. 4
    건조the resulting organic layer was dried on anhydrous sodium carbonate
  5. 5
    여과Thereafter, the organic layer was filtered through silica gel (5 g)
  6. 6
    기타the solvent was removed by evaporation
  7. 7
    기타the resulting residue was purified

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728835uspto-grants-1998_03