Hydrazine → 2'-Hydrazino-2,4'-bipyridine

HRID 465120노트

반응식

HRID 465120 반응식
Cl[C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)[CH:5]=[CH:4][N:3]=1.[NH2:14][NH2:15]>N1C=CC=CC=1>[NH:14]([C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)[CH:5]=[CH:4][N:3]=1)[NH2:15]

참가 물질

4

반응물 2

HCID 9321Hydrazine2회HCID 132987272′-Chloro-2,4′-bipyridine

생성물 1

HCID 135337172'-Hydrazino-2,4'-bipyridine

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 5.0 g of 2'-chloro-2,4'-bipyridine, 5 ml of anhydrous hydrazine and 100 ml of pyridine was refluxed. Additional 5 ml portions of anhydrous hydrazine were added after 18, 36 and 54 hours of refluxing. The solution was then refluxed for an additional 48 hours and the solvent removed under vacuum. The solid was dissolved in methylene chloride, treated with activated carbon, filtered and the filtrate concentrated to dryness. The residue was triturated with hexane, giving crystals which were recrystallized from methylene chloride-hexane, giving 2'-hydrazino-2,4'-bipyridine as yellow crystals, mp 120°-121° C.

후처리

  1. temperaturewas refluxed
  2. temperatureof refluxing
  3. temperatureThe solution was then refluxed for an additional 48 hours
  4. customthe solvent removed under vacuum
  5. dissolutionThe solid was dissolved in methylene chloride
  6. additiontreated with activated carbon
  7. filtrationfiltered
  8. concentrationthe filtrate concentrated to dryness
  9. customThe residue was triturated with hexane
  10. customgiving crystals which
  11. customwere recrystallized from methylene chloride-hexane

출처 및 근거

ORD 기록
ord-7374b81c7b8a4ec48b361259b01a6de6
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04550166

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