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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
ノート
印刷プレビュー

反応式

HRID 352924 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 24085Mercuric Chloride
触媒
HCID 702Ethanol溶媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-fc3a74b8e4e24755ac82eb416493f431
出典データセット
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06747023B1

反応ノート

読み込み中…

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