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

HRID 465120ノート

反応式

HRID 465120 の反応式
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]

参加物

4

反応物 2

HCID 9321Hydrazine2 回HCID 132987272′-Chloro-2,4′-bipyridine

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7374b81c7b8a4ec48b361259b01a6de6
出典データセット
uspto-grants-1985_10
特許番号
US04550166

反応ノート

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