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Piperazine → HCID 19812356, 화합물

HRID 373314
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HRID 373314 반응식
[Cl:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([C:10]2[CH:15]=[CH:14][N+:13]([O-:16])=[CH:12][CH:11]=2)=[CH:4][N:3]=1.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>C(O)C>[ClH:1].[C:8]([C:7]1[C:2]([N:17]2[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]2)=[N:3][CH:4]=[C:5]([C:10]2[CH:15]=[CH:14][N+:13]([O-:16])=[CH:12][CH:11]=2)[CH:6]=1)#[N:9]
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참가 물질

4

반응물 2

HCID 4837PiperazineHCID 10243008HCID 10243008, 화합물

생성물 1

HCID 19812356HCID 19812356, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 2 g 2-chloro-3-cyano-5,4'-bipyridine-1'-oxide, 0.8 g piperazine, 0.52 g of KHCO3 and 80 ml ethanol is refluxed for 3 hours and then evaporated to dryness under vacuum. The residue is dissolved in 10 ml 1N HCl and the solution is mixed with ethanol until crystallization occurs. After cooling overnight, the crystals that are formed are filtered off with suction and dried at 110° C. Yield: 2.23 g (81.2% of the theoretical yield), having a melting point of 255° C.-260° C.

후처리

temperature
is refluxed for 3 hours
  • customevaporated to dryness under vacuum
  • dissolutionThe residue is dissolved in 10 ml 1N HCl
  • additionthe solution is mixed with ethanol until crystallization
  • temperatureAfter cooling overnight
  • customthe crystals that are formed
  • filtrationare filtered off with suction
  • customdried at 110° C
  • customYield: 2.23 g (81.2% of the theoretical yield),
  • 출처 및 근거

    ORD 기록
    ord-e4a215e85e30478db656fbc8b08344c0
    출처 데이터셋
    uspto-grants-1992_11
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05162533

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