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Ammonia → 2-Piperazin-1-yl-benzamide

HRID 276892
ノート
印刷プレビュー

反応式

HRID 276892 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1)#[N:2].N.S(=O)(=O)(O)[OH:17]>>[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1)(=[O:17])[NH2:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 222AmmoniaHCID 1118Sulfuric AcidHCID 2735875N-(2-Cyanophenyl)piperazine

生成物 1

HCID 106558542-Piperazin-1-yl-benzamide

実験手順

1-(2-Cyanophenyl)piperazine (1.8 g, 9.8 mmol) was dissolved in 90% sulfuric acid aqueous solution (20 ml) and stirred at a room temperature for 24 hours. The reaction solution was slowly added dropwise to a mixture of ice (75 g) and 28% aqueous ammonia (75 ml), and the reaction product was extracted with chloroform. The extract was washed with saturated brine and dried with sodium sulfate. Then the compound obtained by the evaporation of the solvent under a reduced pressure was separated by an aluminum column chromatography to obtain colorless crystals. By further recrystallizing the thus obtained crystals from ethyl acetate, 680 mg of the title compound was obtained (3.1 mmol, 32% in yield).

後処理

  • extractionthe reaction product was extracted with chloroform
  • washThe extract was washed with saturated brine
  • dry with materialdried with sodium sulfate
  • customThen the compound obtained by the evaporation of the solvent under a reduced pressure
  • customwas separated by an aluminum column chromatography
  • customto obtain colorless crystals
  • customBy further recrystallizing the thus obtained crystals from ethyl acetate
  • 出典と根拠

    ORDレコード
    ord-de76be4ed8d3435bb3264cc36190c0e7
    出典データセット
    uspto-grants-2002_03
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US06355642B1

    反応ノート

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