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Sulfuryl chloride → N-{2,4-difluoro-3-[1-ethyl-4-(pyridin-4-yl)-1H-pyrazol-3-yl]phenyl}-2,5-difluorobenzenesulfonamide

HRID 1843635
ノート
印刷プレビュー

反応式

HRID 1843635 の反応式
[CH2:1]([N:3]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=2)[C:5]([C:14]2[C:15]([F:22])=[C:16]([NH2:21])[CH:17]=[CH:18][C:19]=2[F:20])=[N:4]1)[CH3:2].[F:23][C:24]1[CH:29]=[CH:28][C:27]([F:30])=[CH:26][C:25]=1[S:31](Cl)(=[O:33])=[O:32].S(Cl)(Cl)(=O)=O>N1C=CC=CC=1>[CH2:1]([N:3]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=2)[C:5]([C:14]2[C:15]([F:22])=[C:16]([NH:21][S:31]([C:25]3[CH:26]=[C:27]([F:30])[CH:28]=[CH:29][C:24]=3[F:23])(=[O:33])=[O:32])[CH:17]=[CH:18][C:19]=2[F:20])=[N:4]1)[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24648Sulfuryl chlorideHCID 27369112,5-Difluorobenzenesulfonyl chlorideHCID 671844933-(1-Ethyl-4-pyridin-4-yl-1H-pyrazol-3-yl)-2,4-difluoro-phenylamine

生成物 1

HCID 44622209N-{2,4-difluoro-3-[1-ethyl-4-(pyridin-4-yl)-1H-pyrazol-3-yl]phenyl}-2,5-difluorobenzenesulfonamide収率 62%

試薬・触媒・溶媒 1

HCID 1049Pyridine
溶媒

反応条件

温度
0 °C

実験手順

3-(1-Ethyl-4-pyridin-4-yl-1H-pyrazol-3-yl)-2,4-difluoro-phenylamine (1.146 g, 3.816 mmol) was dissolved in anhydrous pyridine (30 M) under nitrogen atmosphere and cooled to 0° C. 2,5-Difluoro-benzenesulfonyl chloride (0.513 mL, 3.816 mmol, 1 eq) was added and the mixture was allowed to stir at the same temperature. Further additions of sulfonyl chloride (for a total amount of 0.650 mL) were needed to drive the reaction to completion. The reaction mixture was kept at 0° C. overnight and then it was allowed to reach room temperature. The solvent was removed under reduced pressure and the residue was dissolved in ethyl acetate and washed with NaHCO3 saturated aqueous solution. The organic layer was dried over anhydrous sodium sulfate and evaporated to dryness. The crude product was slurried in methanol at 50° C. for 10 minutes and the solid was filtered and washed with ethyl ether. After drying at 40° C. for 5 hours 1.13 g of the title compound were obtained as a white solid (62% yield).

後処理

  1. customthe reaction to completion
  2. customto reach room temperature
  3. customThe solvent was removed under reduced pressure
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. washwashed with NaHCO3 saturated aqueous solution
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. customevaporated to dryness
  8. waitThe crude product was slurried in methanol at 50° C. for 10 minutes
  9. filtrationthe solid was filtered
  10. washwashed with ethyl ether
  11. dry with materialAfter drying at 40° C. for 5 hours 1.13 g of the title compound

出典と根拠

ORDレコード
ord-509b92615f9a47b9b7e298ef8421820c
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946250B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート