Hydrazine hydrate (1:1) → 6-(4-Fluorophenyl)-4,5-dihydro-3(2H)-pyridazinone

HRID 413303노트

반응식

HRID 413303 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH2:9][CH2:10][C:11]([OH:13])=O)=[CH:4][CH:3]=1.O.[NH2:16][NH2:17]>C(O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH2:9][CH2:10][C:11](=[O:13])[NH:16][N:17]=2)=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 1013593-(4-Fluorobenzoyl)propionic acid

생성물 1

HCID 6058786-(4-Fluorophenyl)-4,5-dihydro-3(2H)-pyridazinone수율 86%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

In a round-bottomed flask, 4-(4-fluoro-phenyl)-4-oxo-butyric acid (4.90 g, 25.0 mmol) and hydrazine hydrate (1.70 ml, 35.0 mmol) were dissolved in ethanol (50 ml), and the reaction mixture was heated to about 80° C. for about ninety minutes. The mixture was allowed to cool to room temperature and then concentrated in vacuo. The resulting solids were suspended and stirred in ethanol (10 ml) for ten minutes and the mixture was then filtered to give pure product (4.14 g, 21.5 mmol, 86% yield). LRMS ([M+H]+)=193.2; m.p. 191-193° C.

후처리

  1. temperatureto cool to room temperature
  2. concentrationconcentrated in vacuo
  3. filtrationthe mixture was then filtered

출처 및 근거

ORD 기록
ord-a9cbcc58b91b4de7bff44c4f7c077059
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06566377B2

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