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3',4',5-Trichlorosalicylanilide → HCID 57756581、化合物

HRID 228639
ノート
印刷プレビュー

反応式

HRID 228639 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[CH:4][CH:3]=1.[Cl:16][C:17]1[CH:18]=[C:19]([CH:31]=[CH:32][C:33]=1[Cl:34])[NH:20][C:21](=[O:30])[C:22]1[C:23](=[CH:25][CH:26]=[C:27]([Cl:29])[CH:28]=1)[OH:24]>CN(C)C1C=CN=CC=1.ClC1C=CC=CC=1Cl>[Cl:16][C:17]1[CH:18]=[C:19]([NH:20][C:21](=[O:30])[C:22]2[CH:28]=[C:27]([Cl:29])[CH:26]=[CH:25][C:23]=2[O:24][C:2]2[C:11]3[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=3)[N:5]=[CH:4][CH:3]=2)[CH:31]=[CH:32][C:33]=1[Cl:34]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 695063',4',5-TrichlorosalicylanilideHCID 4596104-Chloro-6,7-dimethoxyquinoline

生成物 1

HCID 57756581HCID 57756581、化合物収率 6%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 72391,2-Dichlorobenzene溶媒

反応条件

温度
120 °C

実験手順

4-Chloro-6,7-dimethoxyquinoline (116 mg), 3′,4′,5-trichlorosalicylanilide (632 mg), and 4-dimethylaminopyridine (244 mg) were suspended in o-dichlorobenzene (1 ml), and the suspension was stirred at 120° C. overnight. The reaction solution was cooled to room temperature, and the solvent was removed by distillation under the reduced pressure. Water was then added to the residue, and the mixture was extracted with chloroform. The chloroform layer was washed with water and was dried over anhydrous sodium sulfate. The solvent was removed therefrom by distillation under the reduced pressure, and the residue was purified by column chromatography using acetone-hexane to give the title compound (14 mg, yield 6%).

後処理

  1. temperatureThe reaction solution was cooled to room temperature
  2. customthe solvent was removed by distillation under the reduced pressure
  3. additionWater was then added to the residue
  4. extractionthe mixture was extracted with chloroform
  5. washThe chloroform layer was washed with water
  6. dry with materialwas dried over anhydrous sodium sulfate
  7. customThe solvent was removed
  8. distillationby distillation under the reduced pressure
  9. customthe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-db296daa704d4940a71ee953b98a8290
出典データセット
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07560558B2

反応ノート

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