Water → N-{1-[2-(6,7-Dimethoxy-quinolin-4-yloxy)-4,5-dimethyl-phenyl]-ethylidene}-N'-pyridin-2-yl-hydrazine

HRID 228728

반응식

HRID 228728 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[O:15][C:16]1[CH:21]=[C:20]([CH3:22])[C:19]([CH3:23])=[CH:18][C:17]=1[C:24](=O)[CH3:25].[N:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[NH:33][NH2:34].O>C(O)C.[O-]S(C(F)(F)F)(=O)=O.[Yb+3].[O-]S(C(F)(F)F)(=O)=O.[O-]S(C(F)(F)F)(=O)=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[O:15][C:16]1[CH:21]=[C:20]([CH3:22])[C:19]([CH3:23])=[CH:18][C:17]=1[C:24](=[N:34][NH:33][C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][N:27]=1)[CH3:25]

참가 물질

6

반응물 3

HCID 962WaterHCID 786452-HydrazinopyridineHCID 100665381-(2-((6,7-Dimethoxyquinolin-4-yl)oxy)-4,5-dimethylphenyl)ethan-1-one2회

생성물 1

HCID 86605186N-{1-[2-(6,7-Dimethoxy-quinolin-4-yloxy)-4,5-dimethyl-phenyl]-ethylidene}-N'-pyridin-2-yl-hydrazine수율 39%

시약·촉매·용매 2

HCID 2733225Ytterbium triflate촉매HCID 702Ethanol용매

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온도
60 °C

실험 절차

1-[2-(6,7-Dimethoxy-quinolin-4-yloxy)-4,5-dimethylphenyl]-1-ethanone (compound 38) (30 mg) was dissolved in ethanol (1 ml) to prepare a solution. (2-Pyridyl)hydrazine (28 mg) was added to the solution, and the mixture was stirred at 60° C. overnight. Ytterbium triflate (1 mg) was added to the reaction solution, and the mixture was stirred at 60° C. for 5 days. The reaction solution was cooled to room temperature, water was then added to the cooled solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was then washed with water and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure. The residue was purified by thin layer chromatography using hexane-acetone to give the title compound (13 mg, yield 39%).

후처리

  1. customto prepare a solution
  2. stirringthe mixture was stirred at 60° C. for 5 days
  3. temperatureThe reaction solution was cooled to room temperature
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe ethyl acetate layer was then washed with water
  6. dry with materialwas dried over anhydrous sodium sulfate
  7. customThe solvent was removed by distillation under the reduced pressure
  8. customThe residue was purified by thin layer chromatography

출처 및 근거

ORD 기록
ord-7c95e67f377d4b118cc2345292be6415
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560558B2

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