Potassium Carbonate → HCID 86644471, 화합물

HRID 2404540노트

반응식

HRID 2404540 반응식
[C:1]([NH:4][C:5]1[N:9]([C:10]2[CH:15]=[C:14]([S:16][CH2:17][C:18]([F:21])([F:20])[F:19])[C:13]([CH3:22])=[CH:12][C:11]=2[F:23])[N:8]=[C:7]([OH:24])[CH:6]=1)(=[O:3])[CH3:2].[C:25](=O)([O-])[O-].[K+].[K+].[F:31][C:32]([F:55])([F:54])[C:33]([F:53])([F:52])[C:34]([F:51])([F:50])[C:35]([F:49])([F:48])S(OCC(F)(F)C(F)(F)F)(=O)=O>CS(C)=O>[C:1]([NH:4][C:5]1[N:9]([C:10]2[CH:15]=[C:14]([S:16][CH2:17][C:18]([F:19])([F:20])[F:21])[C:13]([CH3:22])=[CH:12][C:11]=2[F:23])[N:8]=[C:7]([O:24][CH2:25][C:35]([F:48])([F:49])[C:34]([F:50])([F:51])[C:33]([F:52])([F:53])[C:32]([F:31])([F:54])[F:55])[CH:6]=1)(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 866246582,2,3,3,3-Pentafluoropropyl nonafluorobutane-1-sulfonateHCID 178474353HCID 178474353, 화합물

생성물 1

HCID 86644471HCID 86644471, 화합물수율 67.1%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

0.5 g of 5-acetylamino-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-hydroxypyrazole was dissolved in 10 mL of dimethylsulfoxide, and 0.23 g of potassium carbonate was added, followed by stirring at room temperature for 5 minutes. To this solution, 0.79 g of 2,2,3,3,3-pentafluoropropyl nonafluorobutanesulfonate was added, followed by stirring at room temperature for 12 hours. Then, extraction with ethyl acetate was carried out, the organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure, and the obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:4) to obtain 0.55 g of 5-acetylamino-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-(2,2,3,3,4,4,5,5,5-nonafluoropentyloxy)pyrazole.

후처리

  1. stirringby stirring at room temperature for 12 hours
  2. extractionThen, extraction with ethyl acetate
  3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customthe obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:4)

출처 및 근거

ORD 기록
ord-a2219ae534c34cd1971d49cd6554683a
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802713B2

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