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Cesium carbonate → HCID 78322475, 화합물

HRID 1053179
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인쇄 미리보기

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HRID 1053179 반응식
[C:1]([O-:4])([O-])=O.[Cs+].[Cs+].F[C:8]1[CH:23]=[CH:22][C:21]([O:24][C:25]([F:28])([F:27])[F:26])=[CH:20][C:9]=1[C:10]([NH:12][C:13]1[CH:18]=[CH:17][NH:16][C:15](=[O:19])[CH:14]=1)=[O:11].[F:29][C:30]1[CH:35]=[CH:34][C:33](O)=[CH:32][C:31]=1C>CN(C=O)C>[F:29][C:30]1[CH:35]=[CH:34][C:1]([O:4][C:8]2[CH:23]=[CH:22][C:21]([O:24][C:25]([F:28])([F:27])[F:26])=[CH:20][C:9]=2[C:10]([NH:12][C:13]2[CH:18]=[CH:17][NH:16][C:15](=[O:19])[CH:14]=2)=[O:11])=[C:32]([CH3:33])[CH:31]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 27373944-Fluoro-3-methylphenolHCID 86728473HCID 86728473, 화합물

생성물 1

HCID 78322475HCID 78322475, 화합물수율 43%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

Cs2CO3 (651.6 mg, 2 mmol) was added to a solution of 2-fluoro-N-(2-oxo-1,2-dihydropyridin-4-yl)-5-(trifluoromethoxy)benzamide (63.2 mg, 0.2 mmol) and 4-fluoro-3-methylphenol (252.3 mg, 2 mmol) in DMF (1 mL) and the reaction was stirred at 100° C. for 1 hours. The reaction was filtered and purified by reverse phase HPLC using a gradient of acetonitrile in water (10-99%) and HCl as a modifier to yield 2-(4-fluoro-2-methylphenoxy)-N-(2-oxo-1,2-dihydropyridin-4-yl)-5-(trifluoromethoxy)benzamide (40) (36.3 mg, 43%). ESI-MS m/z calc. 422.09. found 423.9 (M+1)+; Retention time: 1.64 minutes (3 minutes run).

후처리

  1. filtrationThe reaction was filtered
  2. custompurified by reverse phase HPLC

출처 및 근거

ORD 기록
ord-47ed29866e3440fcb73ea8fc572ac028
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09393235B2

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