Ethyl Acetate → 3-Benzoyl-4-(2-methoxyphenylamino)-8-methoxyquinoline

HRID 1382325ノート

反応式

HRID 1382325 の反応式
C(C1C=NC2C(C=1Cl)=CC=CC=2OC)(=O)C1C=CC=CC=1.[C:22]([C:30]1[CH:31]=[N:32][C:33]2[C:38]([C:39]=1[NH:40][C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][C:42]=1[O:47][CH3:48])=[CH:37][CH:36]=[CH:35][C:34]=2[O:49][CH3:50])(=[O:29])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.C(OCC)(=O)C>O1CCOCC1.COC1C(N)=CC=CC=1>[C:22]([C:30]1[CH:31]=[N:32][C:33]2[C:38]([C:39]=1[NH:40][C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][C:42]=1[O:47][CH3:48])=[CH:37][CH:36]=[CH:35][C:34]=2[O:49][CH3:50])(=[O:29])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

参加物

5

反応物 2

HCID 8857Ethyl AcetateHCID 212745613-benzoyl-4-(2-methoxyphenylamino)-8-methoxyquinoline 3-Benzoyl-4-chloro-8-methoxyquinoline

生成物 1

HCID 212745583-Benzoyl-4-(2-methoxyphenylamino)-8-methoxyquinoline収率 61%

試薬・触媒・溶媒 2

HCID 70002-Methoxyaniline溶媒HCID 312751,4-Dioxane溶媒

実験手順

Preparation of 3-benzoyl-4-(2-methoxyphenylamino)-8-methoxyquinoline 3-Benzoyl-4-chloro-8-methoxyquinoline (2.8 g, 0.0094 mol) was heated under reflux in a mixture of 1,4-dioxan (50 ml) and o-anisidine (7 ml) for 1 hour. The solvent was evaporated and the residue was dissolved in dichloromethane, and washed with dilute hydrochloric acid, sodium hydrogen carbonate solution, water and brine. The organic solution was dried and evaporated to an oil which was chromatographed (silica gel, 1% methanol in dichloromethane) to give an oil which afforded yellow crystals of 3-benzoyl-4-(2-methoxyphenylamino)-8-methoxyquinoline (2.2 g, 61%) from ethyl acetate, m.p. 200°-202°.

後処理

  1. temperaturewas heated
  2. customThe solvent was evaporated
  3. dissolutionthe residue was dissolved in dichloromethane
  4. washwashed with dilute hydrochloric acid, sodium hydrogen carbonate solution, water and brine
  5. customThe organic solution was dried
  6. customevaporated to an oil which
  7. customwas chromatographed (silica gel, 1% methanol in dichloromethane)
  8. customto give an oil which

出典と根拠

ORDレコード
ord-5f51b2bab7174239a6d55b6bda0fd751
出典データセット
uspto-grants-1989_02
特許番号
US04806550

反応ノート

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