反応 #2555

ord-0679f3c83e8041a093c3b3901f299d06

反応方程式

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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度With cooling in an ice bath
  2. 2
    抽出The reaction solution was extracted with ether
  3. 3
    洗浄washed with saturated brine
  4. 4
    乾燥the resulting organic layer was dried on anhydrous sodium carbonate
  5. 5
    ろ過Thereafter, the organic layer was filtered through silica gel (5 g)
  6. 6
    その他the solvent was removed by evaporation
  7. 7
    その他the resulting residue was purified

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05728835uspto-grants-1998_03