Pyridine → HCID 21955570, 화합물

HRID 601644

반응식

HRID 601644 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 21955570HCID 21955570, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d22f9d9a8b7c45eab93dfa0270778f9d
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902369B2

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