Potassium Carbonate → Fruquintinib

HRID 1510821노트

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HRID 1510821 반응식
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][N:3]=1.[OH:16][C:17]1[CH:30]=[CH:29][C:20]2[C:21]([C:25]([NH:27][CH3:28])=[O:26])=[C:22]([CH3:24])[O:23][C:19]=2[CH:18]=1.C([O-])([O-])=O.[K+].[K+]>CC#N>[CH3:13][O:12][C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][C:8]=1[O:14][CH3:15])[N:5]=[CH:4][N:3]=[C:2]2[O:16][C:17]1[CH:30]=[CH:29][C:20]2[C:21]([C:25]([NH:27][CH3:28])=[O:26])=[C:22]([CH3:24])[O:23][C:19]=2[CH:18]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 27693644-Chloro-6,7-dimethoxyquinazolineHCID 167551736-Hydroxy-N,2-dimethylbenzofuran-3-carboxamide

생성물 1

HCID 44480399Fruquintinib수율 85%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 4-chloro-6,7-dimethoxyquinazoline (1 equiv.) in 2 ml CH3CN were added 6-hydroxy-N,2-dimethylbenzofuran-3-carboxamide (1 equiv.) and K2CO3 (1.5 equiv.). The mixture was refluxed under stirring for 10 hr. After the solvent was evaporated, the residue was washed with water, dried over MgSO4, filtered, concentrated, and purified by column chromatography to give the title compound in a yield of 85%.

후처리

  1. temperatureThe mixture was refluxed
  2. customAfter the solvent was evaporated
  3. washthe residue was washed with water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-cda1951738de479d89ba963fdb9784ce
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08212033B2

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