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Azobisisobutyronitrile → [6-(2,5-Difluorobenzoyl)pyridin-3-yl]methyl acetate

HRID 748832
ノート
印刷プレビュー

反応式

HRID 748832 の反応式
BrN1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N.[F:21][C:22]1[CH:27]=[CH:26][C:25]([F:28])=[CH:24][C:23]=1[CH:29]([OH:37])[C:30]1[CH:35]=[CH:34][C:33]([CH3:36])=[CH:32][N:31]=1.S([O-])([O-])(=O)=S.[Na+].[Na+].[C:45]([O-:48])(=[O:47])[CH3:46].[Na+]>C(Cl)(Cl)(Cl)Cl.C(OCC)(=O)C>[C:45]([O:48][CH2:36][C:33]1[CH:32]=[N:31][C:30]([C:29]([C:23]2[CH:24]=[C:25]([F:28])[CH:26]=[CH:27][C:22]=2[F:21])=[O:37])=[CH:35][CH:34]=1)(=[O:47])[CH3:46]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6547AzobisisobutyronitrileHCID 24477Sodium ThiosulfateHCID 67184N-bromobutanimideHCID 517045Sodium AcetateHCID 23114839HCID 23114839、化合物

生成物 1

HCID 23114640[6-(2,5-Difluorobenzoyl)pyridin-3-yl]methyl acetate収率 18.4%

試薬・触媒・溶媒 2

HCID 5943Carbon Tetrachloride溶媒HCID 8857Ethyl Acetate溶媒

実験手順

While heating under reflux, N-bromosuccinimide (6.0 g, 33.6 mmol) and a catalytic amount of 2,2′-azobis(2-methylpropionitrile) were added to a solution of the 2-[(2,5-difluorophenyl)-hydroxymethyl]-5-methylpyridine (2.64 g, 11.2 mmol), which had been obtained in Referential Example 15, in carbon tetrachloride (60 ml). The resulting mixture was then, stirred. After reflux for 7 hours, the reaction mixture was cooled to room temperature and added to an aqueous solution of sodium thiosulfate. The mixture was extracted with ether. The solution was washed with water and brine, and then dried over sodium sulfate. The residue obtained by concentrating the solution under reduced pressure was dissolved in toluene and the resulting solution was concentrated again. The residue was dissolved in N,N-dimethylformamide (20 ml). Sodium acetate (4.59 g, 56 mmol) was added to the resulting solution and the mixture was stirred at 70° C. for 17 hours. After cooling, the reaction mixture was dissolved in ethyl acetate (100 ml), followed by washing with water and brine. The solution was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane:ethyl acetate=5:1) to yield the title compound (600 mg, 18%) as an oil.

後処理

  1. temperatureWhile heating
  2. temperatureunder reflux
  3. temperatureAfter reflux for 7 hours
  4. extractionThe mixture was extracted with ether
  5. washThe solution was washed with water and brine
  6. dry with materialdried over sodium sulfate
  7. customThe residue obtained
  8. concentrationby concentrating the solution under reduced pressure
  9. dissolutionwas dissolved in toluene
  10. concentrationthe resulting solution was concentrated again
  11. dissolutionThe residue was dissolved in N,N-dimethylformamide (20 ml)
  12. stirringthe mixture was stirred at 70° C. for 17 hours
  13. temperatureAfter cooling
  14. washby washing with water and brine
  15. dry with materialThe solution was dried over anhydrous magnesium sulfate
  16. concentrationconcentrated under reduced pressure
  17. customThe residue was purified by silica gel chromatography (hexane:ethyl acetate=5:1)

出典と根拠

ORDレコード
ord-268c71bd663344c8b582f74ff5d83235
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07399775B2

反応ノート

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