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Hydrazine hydrate (1:1) → 2-(2-Methoxy-4-amino-5-nitro-phenyl)-5-methoxy-imidazo[4,5-b]pyridine

HRID 3872
ノート
印刷プレビュー

反応式

HRID 3872 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([N:9]2C(=O)C(C)(C)C3C(=CC([N+]([O-])=O)=CC=3)C2=O)[C:6]([N+:26]([O-:28])=[O:27])=[CH:5][C:4]=1[C:29]1[NH:30][C:31]2[C:32]([N:39]=1)=[N:33][C:34]([O:37][CH3:38])=[CH:35][CH:36]=2.O.NN>C(O)(C)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([NH2:9])[C:6]([N+:26]([O-:28])=[O:27])=[CH:5][C:4]=1[C:29]1[NH:30][C:31]2[C:32]([N:39]=1)=[N:33][C:34]([O:37][CH3:38])=[CH:35][CH:36]=2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 201532782-[2-methoxy-5-nitro-4-(4,4-dimethyl-7-nitro-2H,4H-isoquinolin-1,3-dione-2-yl)-phenyl]-5-methoxy-imidazo[4,5-b]pyridine

生成物 1

HCID 201532722-(2-Methoxy-4-amino-5-nitro-phenyl)-5-methoxy-imidazo[4,5-b]pyridine

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

One half gram of 2-[2-methoxy-5-nitro-4-(4,4-dimethyl-7-nitro-2H,4H-isoquinolin-1,3-dione-2-yl)-phenyl]-5-methoxy-imidazo[4,5-b]pyridine is suspended in 10 ml of isopropanol, mixed with 0.5 ml of 80% hydrazine hydrate, and refluxed for 1.75 hours with stirring. The reaction mixture is concentrated by evaporation, the residue is triturated with 50 ml of ice water, and the product precipitated is purified by chromatography on silica gel [eluant: methylene chloride/ethanol (100:0 to 100:2)].

後処理

  1. temperaturerefluxed for 1.75 hours
  2. concentrationThe reaction mixture is concentrated by evaporation
  3. customthe residue is triturated with 50 ml of ice water
  4. customthe product precipitated
  5. customis purified by chromatography on silica gel [eluant: methylene chloride/ethanol (100:0 to 100:2)]

出典と根拠

ORDレコード
ord-f3d5d152d9a34241b654d7e6361c94bd
出典データセット
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04722929

反応ノート

読み込み中…

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