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

HRID 470833

반응식

HRID 470833 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-0ee7a6fef7114c7a8c6f7c93d64bd6f3
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629167B2

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