Hydrazine → 2-Hydrazino-3,3'-bipyridine

HRID 465113ノート

反応式

HRID 465113 の反応式
Cl[C:2]1[C:7]([C:8]2[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=2)=[CH:6][CH:5]=[CH:4][N:3]=1.[NH2:14][NH2:15]>N1C=CC=CC=1>[NH:14]([C:2]1[C:7]([C:8]2[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=2)=[CH:6][CH:5]=[CH:4][N:3]=1)[NH2:15]

参加物

4

反応物 2

HCID 9321HydrazineHCID 104200582-Chloro-3,3'-bipyridine

生成物 1

HCID 135337152-Hydrazino-3,3'-bipyridine

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
110 °C

実験手順

A 440 mg portion of 2-chloro-3,3'-bipyridine and 0.73 ml of anhydrous hydrazine were dissolved in 15 ml of pyridine and heated at 110° C. for 3 days. The volatiles were removed at reduced pressure, 10 ml of toluene was added and the volatiles again removed. The residue was partitioned between 125 ml of methylene chloride and 25 ml of saturated aqueous sodium carbonate. The organic layer was dried and the solvent removed at reduced pressure, giving an oily solid which was recrystallized from methylene chloride-hexane, giving 2-hydrazino-3,3'-bipyridine as a tan powder, mp 104.5°-107° C.

後処理

  1. customThe volatiles were removed at reduced pressure, 10 ml of toluene
  2. additionwas added
  3. customthe volatiles again removed
  4. customThe residue was partitioned between 125 ml of methylene chloride and 25 ml of saturated aqueous sodium carbonate
  5. customThe organic layer was dried
  6. customthe solvent removed at reduced pressure
  7. customgiving an oily solid which
  8. customwas recrystallized from methylene chloride-hexane

出典と根拠

ORDレコード
ord-502ee92532264767b2575038b721b5b4
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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