4-Hydroxyquinoline → Quinoline

HRID 1534471

반응식

HRID 1534471 반응식
[NH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=O)[CH:3]=[CH:2]1>P(Cl)(Cl)(Cl)=O>[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

참가 물질

3

반응물 1

HCID 691414-Hydroxyquinoline

생성물 1

HCID 7047Quinoline수율 79.4%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

3-butyryl-6-benzoyloxymethyl)-4(1H)-quinolone (30 g) was heated under reflux in phosphorus oxychloride (200 ml) for 30 minutes. The solvent was evaporated and the residue partitioned between dichloromethane and ammonia solution. The organic layer was washed successively with sodium hydrogen carbonate solution and 50% brine. Dried anhyd. MgSO4), filtered and evaporated to an oily solid which crystallized on trituration with petroleum ether to give 3-butyryl-4-chloro-6-benzyloxymethyl)quinoline (21.2 g, 67%), m.p. 85° C.-6° C.

후처리

  1. customThe solvent was evaporated
  2. customthe residue partitioned between dichloromethane and ammonia solution
  3. washThe organic layer was washed successively with sodium hydrogen carbonate solution and 50% brine
  4. customDried
  5. filtrationMgSO4), filtered
  6. customevaporated to an oily solid which
  7. customcrystallized on trituration with petroleum ether

출처 및 근거

ORD 기록
ord-14c173a9bff4469eb6fc04397d1b6174
출처 데이터셋
uspto-grants-1992_02
특허 번호
US05089504

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