Pyridine → HCID 21955570、化合物

HRID 601644

反応式

HRID 601644 の反応式
[F:1][C:2]([F:15])([F:14])[S:3]([O:6]S(C(F)(F)F)(=O)=O)(=[O:5])=[O:4].N1C=CC=CC=1.O[C:23]1[CH:32]=[C:31]2[C:26]([C:27](=[O:33])[CH:28]=[CH:29][O:30]2)=[CH:25][CH:24]=1>O>[F:1][C:2]([F:15])([F:14])[S:3]([O:6][C:23]1[CH:32]=[C:31]2[C:26]([C:27](=[O:33])[CH:28]=[CH:29][O:30]2)=[CH:25][CH:24]=1)(=[O:5])=[O:4]

参加物

5

反応物 3

HCID 1049PyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 54092797-Hydroxy-4-benzopyrone

生成物 1

HCID 21955570HCID 21955570、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Under nitrogen atmosphere, 0.24 ml of trifluoromethansulfonic anhydride was added at 0° C. to 4 ml of pyridine solution with 180 g of 7-hydroxy-4H-chromen-4-one, and the mixture was stirred at room temperature for 5 hours. Water was added to the reaction solution, extracted with chloroform. Chloroform layer was washed with saturated saline solution, and then dried with anhydrous sodium sulfate. After distilling out the solvents under reduced pressure, residues were separated and purified with preparative thin-layer chromatography (chloroform/methanol=10/1) to obtain 83 mg of the above compound as a white solid.

後処理

  1. extractionextracted with chloroform
  2. washChloroform layer was washed with saturated saline solution
  3. dry with materialdried with anhydrous sodium sulfate
  4. distillationAfter distilling out the solvents under reduced pressure, residues
  5. customwere separated
  6. custompurified with preparative thin-layer chromatography (chloroform/methanol=10/1)

出典と根拠

ORDレコード
ord-d22f9d9a8b7c45eab93dfa0270778f9d
出典データセット
uspto-grants-2011_03
特許番号
US07902369B2

関連ノート

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