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Pyridine → HCID 86613921, 화합물

HRID 1811412
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HRID 1811412 반응식
N1C=CC=CC=1.[F:7][C:8]([F:21])([F:20])[S:9]([O:12]S(C(F)(F)F)(=O)=O)(=[O:11])=[O:10].O[C:23]1[CH:32]=[CH:31][C:30]([CH3:33])=[C:29]2[C:24]=1[CH2:25][CH2:26][C:27](=[O:34])[NH:28]2>ClCCl>[CH3:33][C:30]1[CH:31]=[CH:32][C:23]([O:12][S:9]([C:8]([F:21])([F:20])[F:7])(=[O:11])=[O:10])=[C:24]2[C:29]=1[NH:28][C:27](=[O:34])[CH2:26][CH2:25]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 10976036HCID 10976036, 화합물

생성물 1

HCID 86613921HCID 86613921, 화합물수율 97%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Pyridine (6.2 ml) and trifluoromethanesulfonic anhydride (10.3 ml) were added with stirring at 0° C. to an anhydrous dichloromethane solution (30 ml) of 5-hydroxy-8-methyl-3,4-dihydro-1H-quinolin-2-one (9.0 g), followed by stirring for 1 hour. The resulting mixture was concentrated under reduced pressure, water was added to the residue, and extraction with dichloromethane was performed. The extract was washed with water, an aqueous potassium hydrogensulfate solution and water in this order, and dried over anhydrous sodium sulfate. After concentration under reduced pressure, the residue was recrystallized from an ethyl acetate-diisopropyl ether mixed solvent to thereby obtain 28 g (yield: 97%) of 8-methyl-5-trifluoromethanesulfonyloxy-3,4-dihydro-1H-quinolin-2-one as a light brown powder.

후처리

  1. concentrationThe resulting mixture was concentrated under reduced pressure, water
  2. additionwas added to the residue, and extraction with dichloromethane
  3. washThe extract was washed with water
  4. dry with materialan aqueous potassium hydrogensulfate solution and water in this order, and dried over anhydrous sodium sulfate
  5. concentrationAfter concentration under reduced pressure
  6. customthe residue was recrystallized from an ethyl acetate-diisopropyl ether mixed solvent

출처 및 근거

ORD 기록
ord-b11f46d20bf2463cab79e8bad279791d
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362252B2

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