Water → HCID 86644457, 화합물

HRID 2404528노트

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HRID 2404528 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(=O)([O-])[O-].[K+].[K+].FC(F)(C(F)(F)F)C(F)(F)C(S(O[CH2:41][C:42]([F:56])([F:55])[O:43][C:44]([F:54])([F:53])[C:45]([O:48][C:49]([F:52])([F:51])[F:50])([F:47])[F:46])(=O)=O)(F)F.O>CS(C)=O.C(OCC)(=O)C>[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][CH2:41][C:42]([F:55])([F:56])[O:43][C:44]([F:53])([F:54])[C:45]([O:48][C:49]([F:50])([F:51])[F:52])([F:47])[F:46])[CH:6]=1)(=[O:3])[CH3:2]

참가 물질

7

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 86644458HCID 86644458, 화합물HCID 178474353HCID 178474353, 화합물

생성물 1

HCID 86644457HCID 86644457, 화합물수율 77.6%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 8857Ethyl Acetate용매

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 0.28 g of potassium carbonate and 1.0 g of 2,2-difluoro-2-{2-trifluoromethoxy-(1,1,2,2-tetrafluoroethoxy)}ethyl nonafluorobutylsulfonate were added, followed by stirring at room temperature for 12 hours. After completion of the reaction, the reaction solution was poured into water, extraction with ethyl acetate was carried out, and after washing with a saturated salt solution, 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 (ethyl acetate:hexane=1:4) to obtain 0.67 g of 5-acetylamino-3-[2,2-difluoro-2-{2-trifluoromethoxy-(1,1,2,2-tetrafluoroethoxy)}ethoxy]-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}pyrazole.

후처리

  1. customAfter completion of the reaction
  2. washafter washing with a saturated salt solution
  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 (ethyl acetate:hexane=1:4)

출처 및 근거

ORD 기록
ord-f9696951b94a48298e6f7dd3529c4805
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802713B2

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