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Hydroxyamine hydrochloride → 1-[(5-Chloroindol-2-yl)sulfonyl]-4-[(hydroxyimino)[5-(pyridin-4-yl)pyrimidin-2-yl]methyl]piperazine

HRID 352924
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HRID 352924 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6]([S:11]([N:14]1[CH2:19][CH2:18][N:17]([C:20]([C:22]3[N:27]=[CH:26][C:25]([C:28]4[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=4)=[CH:24][N:23]=3)=S)[CH2:16][CH2:15]1)(=[O:13])=[O:12])=[CH:5]2.Cl.[NH2:35][OH:36].C([O-])(=O)C.[Na+]>C(O)C.[Hg](Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6]([S:11]([N:14]1[CH2:19][CH2:18][N:17]([C:20](=[N:35][OH:36])[C:22]3[N:27]=[CH:26][C:25]([C:28]4[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=4)=[CH:24][N:23]=3)[CH2:16][CH2:15]1)(=[O:13])=[O:12])=[CH:5]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 865920861-[(5-Chloroindol-2-yl)sulfonyl]-4-[[5-(pyridin-4-yl)pyrimidin-2-yl]thiocarbonyl]piperazine

생성물 1

HCID 1363764391-[(5-Chloroindol-2-yl)sulfonyl]-4-[(hydroxyimino)[5-(pyridin-4-yl)pyrimidin-2-yl]methyl]piperazine

시약·촉매·용매 2

HCID 24085Mercuric Chloride
촉매
HCID 702Ethanol용매

실험 절차

In ethanol (50 ml) was suspended 1-[(5-chloroindol-2-yl)sulfonyl]-4-[[5-(pyridin-4-yl)pyrimidin-2-yl]thiocarbonyl]piperazine (243 mg) at room temperature, followed by the successive addition of hydroxylamine hydrochloride (338 mg), sodium acetate (399 mg) and mercury (II) chloride (132 mg). The resulting mixture was stirred at room temperature for 6 hours. The insoluble matter was filtered off through Celite filtration. The residue was purified by chromatography on a silica gel column (7% methanol—methylene chloride), whereby two fractions were obtained. They were concentrated, respectively, whereby a low-polarity compound (20 mg, colorless powder) and a high-polarity compound (20 mg, colorless powder) were obtained. Low-polarity compound:

후처리

  1. customat room temperature
  2. filtrationThe insoluble matter was filtered off through Celite filtration
  3. customThe residue was purified by chromatography on a silica gel column (7% methanol—methylene chloride)
  4. customwhereby two fractions were obtained
  5. concentrationThey were concentrated
  6. customrespectively, whereby a low-polarity compound (20 mg, colorless powder) and a high-polarity compound (20 mg, colorless powder) were obtained

출처 및 근거

ORD 기록
ord-fc3a74b8e4e24755ac82eb416493f431
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06747023B1

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