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Hydrazine hydrate (1:1) → (4-(4-fluoro-phenoxy)-6-(pyridin-3-yloxy)-1H-benzimidazol-2-yl)-hydrazine

HRID 13251
ノート
印刷プレビュー

反応式

HRID 13251 の反応式
O.[NH2:2][NH2:3].[F:4][C:5]1[CH:28]=[CH:27][C:8]([O:9][C:10]2[C:18]3[N:17]=[C:16](S)[NH:15][C:14]=3[CH:13]=[C:12]([O:20][C:21]3[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=3)[CH:11]=2)=[CH:7][CH:6]=1>C(OCC)(=O)C>[F:4][C:5]1[CH:28]=[CH:27][C:8]([O:9][C:10]2[C:18]3[N:17]=[C:16]([NH:2][NH2:3])[NH:15][C:14]=3[CH:13]=[C:12]([O:20][C:21]3[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=3)[CH:11]=2)=[CH:7][CH:6]=1
参加物反応条件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 178505885HCID 178505885、化合物

生成物 1

HCID 23145521(4-(4-fluoro-phenoxy)-6-(pyridin-3-yloxy)-1H-benzimidazol-2-yl)-hydrazine

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
130 °C

実験手順

1.0 ml of hydrazine monohydrate was added to 130 mg of 4-(4-fluoro-phenoxy)-6-(pyridin-3-yloxy)-1H-benzimidazole-2-thiol, and the reaction liquid was stirred overnight at 130° C. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline in order, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), hexane/ethyl acetate=1/1) to obtain the entitled compound.

後処理

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. washwashed with water and saturated saline in order
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. customthe resulting residue was purified
  7. customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), hexane/ethyl acetate=1/1)
  8. customto obtain the entitled compound

出典と根拠

ORDレコード
ord-12857ac82c7d493aadeffb817d916421
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07728025B2

反応ノート

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