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Piperazine → HCID 14459477, 화합물

HRID 1031477
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HRID 1031477 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:10]([CH3:16])[CH2:11][C:12](=[O:15])[NH:13][N:14]=2)[CH:5]=[CH:6][C:7]=1F.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>ClCCl>[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:10]([CH3:16])[CH2:11][C:12](=[O:15])[NH:13][N:14]=2)[CH:5]=[CH:6][C:7]=1[N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1
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참가 물질

4

반응물 2

HCID 4837PiperazineHCID 144594596-(3,4-difluorophenyl)-4,5-dihydro-5-methyl-3(2H)-pyridazinone

생성물 1

HCID 14459477HCID 14459477, 화합물수율 54.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

5.0 g (22.3 mmol) of 6-(3,4-difluorophenyl)-4,5-dihydro-5-methyl-3(2H)-pyridazinone and 19.2 g (222 mmol) of piperazine are stirred at 160° C. for 15 hours. When the reaction mixture has cooled down, it is taken up with 200 ml of dichloromethane and washed with 3×30 ml of water. After drying, the organic phase is concentrated by evaporation and the residue is crystallized with methanol. The solid obtained is suction filtered and recrystallized from ethyl acetate. 3.5 g (54%) of colourless crystals, m.p. 172°-174° C., are obtained.

후처리

  1. temperatureWhen the reaction mixture has cooled down
  2. washwashed with 3×30 ml of water
  3. customAfter drying
  4. concentrationthe organic phase is concentrated by evaporation
  5. customthe residue is crystallized with methanol
  6. customThe solid obtained
  7. filtrationfiltered
  8. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-98d6ad96491b45f4b45f99249944ed8f
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04954501

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