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Piperazine → HCID 14128502, 화합물

HRID 569973
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HRID 569973 반응식
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:7]=1[CH2:8][CH2:9][C:10](=[O:16])[NH:11]2.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C([O-])(O)=O.[Na+]>>[N:17]1([CH2:2][CH2:3][CH2:4][O:5][C:6]2[CH:15]=[CH:14][CH:13]=[C:12]3[C:7]=2[CH2:8][CH2:9][C:10](=[O:16])[NH:11]3)[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 4837PiperazineHCID 516892Sodium BicarbonateHCID 12899139HCID 12899139, 화합물

생성물 1

HCID 14128502HCID 14128502, 화합물

실험 절차

(a)-1 3.0 Grams of 5-(3-chloropropoxy)-3,4-dihydrocarbostyril, 10 g of piperazine are mixed with 20 ml of hexamethylphosphoryl triamide and heated at 80°-90° C. for 5 hours. The reaction mixture is distilled under a reduced pressure to remove hexamethylphosphoryl triamide and unreacted piperazine. To the residue thus obtained are added 30 ml of 5%-NaHCO3 aqueous solution, followed by extraction with chloroform. The chloroform layer is washed with water and chloroform is removed by distillation. The residue thus obtained is purified by silica-gel chromatography to obtain 1.8 g of 5-(3-piperazinylpropoxy)-3,4-dihydrocarbostyril having a melting point of 192°-195° C.

후처리

  • temperatureheated at 80°-90° C. for 5 hours
  • distillationThe reaction mixture is distilled under a reduced pressure
  • customto remove hexamethylphosphoryl triamide and unreacted piperazine
  • customTo the residue thus obtained
  • extractionfollowed by extraction with chloroform
  • washThe chloroform layer is washed with water and chloroform
  • customis removed by distillation
  • customThe residue thus obtained
  • customis purified by silica-gel chromatography
  • 출처 및 근거

    ORD 기록
    ord-410b0b82f02049d8970a398e3d46a7ca
    출처 데이터셋
    uspto-grants-1988_03
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04734416

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