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Ammonia → 2-Piperazin-1-yl-benzamide

HRID 276892
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HRID 276892 반응식
[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]
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참가 물질

4

반응물 3

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

생성물 1

HCID 106558542-Piperazin-1-yl-benzamide

실험 절차

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).

후처리

  1. extractionthe reaction product was extracted with chloroform
  2. washThe extract was washed with saturated brine
  3. dry with materialdried with sodium sulfate
  4. customThen the compound obtained by the evaporation of the solvent under a reduced pressure
  5. customwas separated by an aluminum column chromatography
  6. customto obtain colorless crystals
  7. customBy further recrystallizing the thus obtained crystals from ethyl acetate

출처 및 근거

ORD 기록
ord-de76be4ed8d3435bb3264cc36190c0e7
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06355642B1

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