反応 #5086

ord-15280f38c7e244d1bfa07303e59094ac

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出the reaction mixture was extracted with 100 ml of ethyl acetate
  2. 2
    洗浄the extract was washed 5 times with 100 ml of water
  3. 3
    乾燥dried with anhydrous magnesium sulfate
  4. 4
    その他The solvent was removed by evaporation
  5. 5
    その他to obtain the residue which
  6. 6
    その他was purified by means of a silica gel column chromatography (eluent: ethyl acetate: n-hexane=1:1)

実験手順

To a mixture of 1.50 g of 4-(3-chlorophenyl)-piperazine and 0.31 g of sodium hydride was added 2.4 ml of epichlorohydrin and the reaction mixture as stirred at room temperature for 30 minutes. After the reaction was completed, the reaction mixture was extracted with 100 ml of ethyl acetate, and the extract was washed 5 times with 100 ml of water, then dried with anhydrous magnesium sulfate. The solvent was removed by evaporation to obtain the residue which was purified by means of a silica gel column chromatography (eluent: ethyl acetate: n-hexane=1:1) to obtain 1.66 g of 4-(3-chlorophenyl)-1-(2,3-epoxypropyl)piperazine as in the form of an oily substance.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05242919uspto-grants-1993_09