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Hydrazine hydrate (1:1) → 2-Hydrazinyl-6-methylpyridine

HRID 498066
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HRID 498066 반응식
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[N:3]=1.O.[NH2:10][NH2:11]>>[NH:10]([C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[N:3]=1)[NH2:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 876016-Chloro-2-picoline

생성물 1

HCID 135904652-Hydrazinyl-6-methylpyridine수율 63.4%

실험 절차

A mixture of 2-chloro-6-methylpyridine (50.6 g, 397 mmol) and hydrazine hydrate (80 mL, 1.65 mol) was heated under reflux for 20 hours. The reaction solution was allowed to cool to room temperature, and excess hydrazine hydrate was evaporated under reduced pressure, and the residue was poured into water. The solution was made basic by the addition of a sodium hydroxide solution, and the organic matter was extracted with chloroform. The extract was washed with saturated brine and water, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue thus obtained was chilled to crystallize, and the resulting crystals were washed with petroleum ether to give the title compound (31.0 g, 63% yield).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 20 hours
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
custom
excess hydrazine hydrate was evaporated under reduced pressure
  • additionthe residue was poured into water
  • additionThe solution was made basic by the addition of a sodium hydroxide solution
  • extractionthe organic matter was extracted with chloroform
  • washThe extract was washed with saturated brine and water
  • dry with materialdried over anhydrous magnesium sulfate
  • customthe solvent was evaporated under reduced pressure
  • customThe residue thus obtained
  • temperaturewas chilled
  • customto crystallize
  • washthe resulting crystals were washed with petroleum ether
  • 출처 및 근거

    ORD 기록
    ord-699191f784344183841dba047a68b569
    출처 데이터셋
    uspto-grants-2005_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06949648B2

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