Dimethylformamide → 4-(4-fluoro-phenoxy)-6-(pyridin-3-yloxy)-2-[1,2,4]triazol-1-yl-1H-benzimidazole

HRID 13254노트

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HRID 13254 반응식
[H-].[Na+].CN(C)C=O.[F:8][C:9]1[CH:35]=[CH:34][C:12]([O:13][C:14]2[C:22]3[N:21]=[C:20](S(C)(=O)=O)[NH:19][C:18]=3[CH:17]=[C:16]([O:27][C:28]3[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=3)[CH:15]=2)=[CH:11][CH:10]=1.[NH:36]1[CH:40]=[N:39][CH:38]=[N:37]1>C(OCC)(=O)C>[F:8][C:9]1[CH:35]=[CH:34][C:12]([O:13][C:14]2[C:22]3[N:21]=[C:20]([N:36]4[CH:40]=[N:39][CH:38]=[N:37]4)[NH:19][C:18]=3[CH:17]=[C:16]([O:27][C:28]3[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=3)[CH:15]=2)=[CH:11][CH:10]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 92571H-1,2,4-TriazoleHCID 24758Sodium hydrideHCID 231453394-(4-fluoro-phenoxy)-2-methanesulfonyl-6-(pyridin-3-yloxy)-1H-benzimidazole

생성물 1

HCID 231453364-(4-fluoro-phenoxy)-6-(pyridin-3-yloxy)-2-[1,2,4]triazol-1-yl-1H-benzimidazole

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
160 °C

실험 절차

5.0 mg of sodium hydride was added to a dimethylformamide (0.5 ml) solution of 16 mg of 4-(4-fluoro-phenoxy)-2-methanesulfonyl-6-(pyridin-3-yloxy)-1H-benzimidazole, and then 10.4 mg of [1,2,4]triazole was added to it, and the reaction liquid was stirred overnight at 160° C. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline in order, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), ethyl acetate) to obtain the entitled compound.

후처리

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. washwashed with water and saturated saline in order
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. customthe resulting residue was purified
  7. customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), ethyl acetate)
  8. customto obtain the entitled compound

출처 및 근거

ORD 기록
ord-5739102b7b02496e84958cd0c1d66046
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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