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

HRID 465113노트

반응식

HRID 465113 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 135337152-Hydrazino-3,3'-bipyridine

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
110 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-502ee92532264767b2575038b721b5b4
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04550166

반응 노트

불러오는 중…