Water → 4-(2-Benzylphenoxy)-6,7-dimethoxyquinoline

HRID 228506

反応式

HRID 228506 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.[CH2:16]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[OH:29])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.O>ClC1C=CC=CC=1Cl>[CH2:16]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[O:29][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)[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

参加物

5

反応物 3

HCID 962WaterHCID 242162-BenzylphenolHCID 4596104-Chloro-6,7-dimethoxyquinoline

生成物 1

HCID 102486464-(2-Benzylphenoxy)-6,7-dimethoxyquinoline収率 10.5%

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

反応条件

温度
180 °C

実験手順

4-Chloro-6,7-dimethoxyquinoline (230 mg) and 2-benzylphenol (254 mg) were suspended in o-dichlorobenzene (1 ml), and the suspension was stirred at 180° C. overnight. The reaction solution was cooled to room temperature, and water was added thereto. The mixture was extracted with ethyl acetate. The ethyl acetate layer was then washed with water and saturated brine and was dried over anhydrous sodium sulfate. The solvent was then removed therefrom by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using ethyl acetate-hexane to give the title compound (40 mg, yield 10%).

後処理

  1. temperatureThe reaction solution was cooled to room temperature
  2. extractionThe mixture was extracted with ethyl acetate
  3. washThe ethyl acetate layer was then washed with water and saturated brine
  4. dry with materialwas dried over anhydrous sodium sulfate
  5. customThe solvent was then removed
  6. distillationby distillation under the reduced pressure
  7. customthe residue was purified by thin layer chromatography

出典と根拠

ORDレコード
ord-b673edf011e34979bd06c6751dc1907b
出典データセット
uspto-grants-2009_07
特許番号
US07560558B2

関連ノート

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