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Ethanol → 1-[(5-Chloroindol-2-yl)sulfonyl]-4-[(hydrazono)[5-(pyridin-4-yl)pyrimidin-2-yl]methyl]piperazine

HRID 352925
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인쇄 미리보기

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HRID 352925 반응식
C(O)C.[Cl:4][C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[NH:10][C:9]([S:14]([N:17]1[CH2:22][CH2:21][N:20]([C:23]([C:25]3[N:30]=[CH:29][C:28]([C:31]4[CH:36]=[CH:35][N:34]=[CH:33][CH:32]=4)=[CH:27][N:26]=3)=S)[CH2:19][CH2:18]1)(=[O:16])=[O:15])=[CH:8]2.O.[NH2:38][NH2:39]>[Hg](Cl)Cl.C(Cl)Cl>[Cl:4][C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[NH:10][C:9]([S:14]([N:17]1[CH2:22][CH2:21][N:20]([C:23](=[N:38][NH2:39])[C:25]3[N:30]=[CH:29][C:28]([C:31]4[CH:36]=[CH:35][N:34]=[CH:33][CH:32]=4)=[CH:27][N:26]=3)[CH2:19][CH2:18]1)(=[O:16])=[O:15])=[CH:8]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)HCID 865920861-[(5-Chloroindol-2-yl)sulfonyl]-4-[[5-(pyridin-4-yl)pyrimidin-2-yl]thiocarbonyl]piperazine

생성물 1

HCID 698815601-[(5-Chloroindol-2-yl)sulfonyl]-4-[(hydrazono)[5-(pyridin-4-yl)pyrimidin-2-yl]methyl]piperazine수율 6,899.4%

시약·촉매·용매 2

HCID 24085
Mercuric Chloride
촉매
HCID 6344Dichloromethane용매

실험 절차

In a mixed solvent of ethanol (100 ml) and methylene chloride (100 ml) was suspended 1-[(5-chloroindol-2-yl)sulfonyl]-4-[[5-(pyridin-4-yl)pyrimidin-2-yl]thiocarbonyl]piperazine (499 mg) at room temperature, followed by the successive addition of hydrazine monohydrate (146 μg) and mercury (II) chloride (272 mg). The resulting mixture was stirred at room temperature for 4 hours. After the solvent was distilled off, the residue was purified by chromatography on a silica gel column (8% methanol—methylene chloride). Methylene chloride was added and the resulting mixture was concentrated. Yellow crystals thus precipitated were collected by filtration and dried, whereby the title compound (100 mg) was obtained.

후처리

  1. customat room temperature
  2. distillationAfter the solvent was distilled off
  3. customthe residue was purified by chromatography on a silica gel column (8% methanol—methylene chloride)
  4. additionMethylene chloride was added
  5. concentrationthe resulting mixture was concentrated
  6. customYellow crystals thus precipitated
  7. filtrationwere collected by filtration
  8. customdried

출처 및 근거

ORD 기록
ord-a7287d15f3c34f13943f113b5aed707c
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06747023B1

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