4-Methylpyridine → 4,4'-Dimethyl-2,2'-bipyridine

HRID 1081230

반응식

HRID 1081230 반응식
[N:1]1[CH:6]=[CH:5][C:4]([CH3:7])=[CH:3][CH:2]=1>[Pd].C1C=CC=CC=1>[CH3:7][C:4]1[CH:5]=[CH:6][N:1]=[C:2]([C:2]2[CH:3]=[C:4]([CH3:7])[CH:5]=[CH:6][N:1]=2)[CH:3]=1

참가 물질

4

반응물 1

HCID 79634-Methylpyridine

생성물 1

HCID 143384,4'-Dimethyl-2,2'-bipyridine

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 241Benzene용매

실험 절차

Freshly distilled 4-picoline (600 ml) was refluxed with palladium on carbon 10% (w/w) for five days. The mixture was then refluxed for a further hour after addition of 100 ml of hot benzene. The palladium on carbon was then removed by filtration (glass-fibre paper). The filtration was repeated until a clear yellow solution was obtained. The volume of the solution was reduced by rotary evaporation to about 200 ml. and was left to stand for 24 hours. White crystals appeared which, after collection, were recrystalised from ethyl acetate. A colourless solid was recovered.

후처리

  1. temperatureThe mixture was then refluxed for a further hour
  2. customThe palladium on carbon was then removed by filtration (glass-fibre paper)
  3. filtrationThe filtration
  4. customwas obtained
  5. customThe volume of the solution was reduced by rotary evaporation to about 200 ml
  6. waitand was left
  7. customafter collection
  8. customwere recrystalised from ethyl acetate
  9. customA colourless solid was recovered

출처 및 근거

ORD 기록
ord-cf304c59b9324b78898d62d2ce935bc0
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05585279

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