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Hydrazine hydrate (1:1) → HCID 16641866、化合物

HRID 1023529
ノート
印刷プレビュー

反応式

HRID 1023529 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[O:9][C:10]1[CH:15]=[CH:14][C:13]([N+:16]([O-])=O)=[CH:12][N:11]=1.O.NN>C(O)C.[Pd]>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[O:9][C:10]1[N:11]=[CH:12][C:13]([NH2:16])=[CH:14][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 24623396HCID 24623396、化合物2 回

生成物 1

HCID 16641866HCID 16641866、化合物収率 88.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

2-[(2,5-dimethylphenyl)oxy]-5-nitropyridine (Intermediate 33, 140 mg, 0.450 mmol) was dissolved in ethanol (3 mL). Hydrazine hydrate (83 μL, 0.884 mmol) and palladium on carbon (47 mg, 0.044 mmol) were added. The reaction mixture was heated at reflux under argon. After overnight heating, the reaction was cooled down. The reaction mixture was filtered. The organic phase was evaporated under vacuum. The residue was purified by SCX (wash with MeOH, desorbed with 2N methanolic ammonia). Evaporation afforded the title compound (85 mg).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux under argon
  3. temperatureAfter overnight heating
  4. temperaturethe reaction was cooled down
  5. filtrationThe reaction mixture was filtered
  6. customThe organic phase was evaporated under vacuum
  7. customThe residue was purified by SCX (wash with MeOH, desorbed with 2N methanolic ammonia)
  8. customEvaporation

出典と根拠

ORDレコード
ord-15e424a75c92465cac059aff32d64a8c
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722695B2

反応ノート

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