4-Hydroxyquinoline → Quinoline

HRID 1534471

反応式

HRID 1534471 の反応式
[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

参加物

3

反応物 1

HCID 691414-Hydroxyquinoline

生成物 1

HCID 7047Quinoline収率 79.4%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-14c173a9bff4469eb6fc04397d1b6174
出典データセット
uspto-grants-1992_02
特許番号
US05089504

関連ノート

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