2'-Hydroxy-4',5'-dimethylacetophenone → HCID 57756422, 화합물

HRID 228908노트

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HRID 228908 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 57756422HCID 57756422, 화합물수율 51.4%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 72391,2-Dichlorobenzene용매

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온도
130 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-859197e649ea4668a1137e8974515726
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560558B2

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