Hydrazine hydrate (1:1) → 4-(1H-Pyrazol-1-yl)benzohydrazide

HRID 470833

反応式

HRID 470833 の反応式
[N:1]1([C:6]2[CH:16]=[CH:15][C:9]([C:10](OCC)=[O:11])=[CH:8][CH:7]=2)[CH:5]=[CH:4][CH:3]=[N:2]1.O.[NH2:18][NH2:19]>CCO>[N:1]1([C:6]2[CH:16]=[CH:15][C:9]([C:10]([NH:18][NH2:19])=[O:11])=[CH:8][CH:7]=2)[CH:5]=[CH:4][CH:3]=[N:2]1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 973146Ethyl 4-(1H-pyrazol-1-YL)benzoate

生成物 1

HCID 432366724-(1H-Pyrazol-1-yl)benzohydrazide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of ethyl 4-(1H-pyrazol-1-yl)benzoate (711 mg, 3.29 mmol) in absolute EtOH (50 mL) was added hydrazine monohydrate (1.6 mL, 32.9 mmol) at room temperature. The reaction mixture was heated to reflux and stirred for 6 d, then concentrated under reduced pressure. The residue was suspended in H2O (30 mL), filtered, washed with H2O (2×20 mL) and EtOH (2×20 mL) to provide the title compound as an off white solid (101 mg, 15%): 1H NMR (400 MHz, CDCl3, δ in ppm) 9.84 (s, 1H), 8.62-8.59 (m, 1H), 7.98-7.90 (m, 4H), 7.81-7.78 (m, 1H), 6.61-6.57 (m, 1H), 4.51 (br d, J=3.3 Hz, 2H).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux
  3. concentrationconcentrated under reduced pressure
  4. filtrationfiltered
  5. washwashed with H2O (2×20 mL) and EtOH (2×20 mL)

出典と根拠

ORDレコード
ord-0ee7a6fef7114c7a8c6f7c93d64bd6f3
出典データセット
uspto-grants-2014_01
特許番号
US08629167B2

関連ノート

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