2'-Hydroxy-4',5'-dimethylacetophenone → HCID 57756422、化合物

HRID 228908ノート

反応式

HRID 228908 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]([CH3:10])=[O:9])[C:5]([OH:11])=[CH:4][C:3]=1[CH3:12].[CH2:13]([O:20][C:21]1[CH:30]=[C:29]2[C:24]([C:25](Cl)=[CH:26][CH:27]=[N:28]2)=[CH:23][C:22]=1[O:32][CH3:33])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>CN(C)C1C=CN=CC=1.ClC1C=CC=CC=1Cl>[CH2:13]([O:20][C:21]1[CH:30]=[C:29]2[C:24]([C:25]([O:11][C:5]3[CH:4]=[C:3]([CH3:12])[C:2]([CH3:1])=[CH:7][C:6]=3[C:8](=[O:9])[CH3:10])=[CH:26][CH:27]=[N:28]2)=[CH:23][C:22]=1[O:32][CH3:33])[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

参加物

5

反応物 2

HCID 1189762'-Hydroxy-4',5'-dimethylacetophenoneHCID 226465627-(Benzyloxy)-4-chloro-6-methoxyquinoline

生成物 1

HCID 57756422HCID 57756422、化合物収率 51.4%

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
130 °C

実験手順

2-Hydroxy-4,5-dimethylacetophenone (3.63 g), 7-benzyloxy-4-chloro-6-methoxyquinoline (1.50 g), and 4-dimethylaminopyridine (2.71 g) were suspended in o-dichlorobenzene (15 ml), and the suspension was stirred at 130° C. overnight. The reaction solution was cooled to room temperature, and the solvent was then removed by distillation under the reduced pressure. Water was added to the residue, and the mixture was extracted with chloroform, and the chloroform layer was then washed with water and saturated brine and was dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using acetone-hexane to give the title compound (1.10 g, yield 37%).

後処理

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

出典と根拠

ORDレコード
ord-859197e649ea4668a1137e8974515726
出典データセット
uspto-grants-2009_07
特許番号
US07560558B2

反応ノート

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