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3-Acetylpyridine → 1-(3-Pyridinyl)-1-ethanone hydrazone

HRID 428951
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인쇄 미리보기

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HRID 428951 반응식
[C:1]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1)(=O)[CH3:2].O.O.[NH2:12][NH2:13]>O>[N:6]1[CH:7]=[CH:8][CH:9]=[C:4]([C:1](=[N:12][NH2:13])[CH3:2])[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 95893-AcetylpyridineHCID 22141362Hydrazine--water (1/2)

생성물 1

HCID 598980421-(3-Pyridinyl)-1-ethanone hydrazone수율 80%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 3-acetylpyridine (6.1 g, 52 mmol) in industrial methylated spirits (50 ml) was added dropwise hydrazine hydrate monohydrate (3.11 ml, 0.1 mol). The reaction mixture was refluxed for 4 h, before cooling to room temperature and stirring for 16 h. Water (25 ml) was added and the volatile organics were removed in vacuo. The predominantly aqueous residual liquor was extracted with ethyl acetate, and the combined organic extracts were dried (Na2SO4) and concentrated to give a yellow oil (5.4 g, 80%) which was taken forward without further purification.

후처리

  1. temperatureThe reaction mixture was refluxed for 4 h
  2. customthe volatile organics were removed in vacuo
  3. extractionThe predominantly aqueous residual liquor was extracted with ethyl acetate
  4. dry with materialthe combined organic extracts were dried (Na2SO4)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-038c360d8d524b7cae77a7c6c57cefe8
출처 데이터셋
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06313312B1

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