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3-Acetylpyridine → 1-[[[[1-(3-Pyridinyl)ethylidene]hydrazino]carbonyl]-methyl]pyridinium chloride

HRID 1111124
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반응식

HRID 1111124 반응식
[CH:1]1[CH:6]=[CH:5][N+:4]([CH2:7][C:8]([NH:10][NH2:11])=[O:9])=[CH:3][CH:2]=1.[Cl-:12].[C:13]([C:16]1[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=1)(=O)[CH3:14]>CO>[Cl-:12].[N:18]1[CH:19]=[CH:20][CH:21]=[C:16]([C:13](=[N:11][NH:10][C:8]([CH2:7][N+:4]2[CH:3]=[CH:2][CH:1]=[CH:6][CH:5]=2)=[O:9])[CH3:14])[CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 95893-AcetylpyridineHCID 70773Pyridinioacetohydrazide chloride

생성물 1

HCID 718323881-[[[[1-(3-Pyridinyl)ethylidene]hydrazino]carbonyl]-methyl]pyridinium chloride수율 71%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To 5.63 gm (0.03 mole) of Girard's Reagent P in 50 ml of anhydrous methanol is added 3.63 gm (0.03 mole) of 3-acetylpyridine. The solution is refluxed 3 hr and cooled. The solvent is evaporated The residue is slurried in 100 ml of anhydrous ether and filtered. The crude product is recrystallized from absolute ethanol to afford 6.18 gm (71%) of the title compound; mp 237.2° (decomp).

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후처리

  1. temperatureThe solution is refluxed 3 hr
  2. temperaturecooled
  3. customThe solvent is evaporated The residue
  4. filtrationfiltered
  5. customThe crude product is recrystallized from absolute ethanol

출처 및 근거

ORD 기록
ord-41d40e258f2e4ec4a80ef8cf8090796f
출처 데이터셋
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04978670

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