m-Chloroperbenzoic acid → HCID 86644468, 화합물

HRID 2404537노트

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HRID 2404537 반응식
[Cl:1][C:2]1[C:3]([O:22][C:23]([F:31])([F:30])[CH:24]([F:29])[C:25]([F:28])([F:27])[F:26])=[N:4][N:5]([C:8]2[CH:13]=[C:12]([S:14][CH2:15][C:16]([F:19])([F:18])[F:17])[C:11]([CH3:20])=[CH:10][C:9]=2[F:21])[C:6]=1[NH2:7].ClC1C=CC=C(C(OO)=[O:40])C=1>C(Cl)(Cl)Cl>[NH2:7][C:6]1[N:5]([C:8]2[CH:13]=[C:12]([S:14]([CH2:15][C:16]([F:19])([F:18])[F:17])=[O:40])[C:11]([CH3:20])=[CH:10][C:9]=2[F:21])[N:4]=[C:3]([O:22][C:23]([F:30])([F:31])[CH:24]([F:29])[C:25]([F:26])([F:27])[F:28])[C:2]=1[Cl:1]

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 86644467HCID 86644467, 화합물

생성물 1

HCID 86644468HCID 86644468, 화합물수율 77.5%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

0.3 g of 4-chloro-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-(1,1,2,3,3,3-hexafluoropropoxy)-5-aminopyrazole was dissolved in 10 mL of chloroform, and 140 mg of m-chloroperbenzoic acid (purity: 75%) was added under cooling with ice. After stirring for one hour under cooling with ice, the solution was washed with an aqueous sodium thiosulfate solution and then washed with an aqueous sodium hydrogen carbonate solution, and then dried over anhydrous sodium sulfate. Then, the solvent was distilled off under reduced pressure, and the obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:2) to obtain 0.24 g of 5-amino-4-chloro 1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylsulfinyl)phenyl}-3-(1,1,2,3,3,3-hexafluoropropoxy)pyrazole.

후처리

  1. temperatureunder cooling with ice
  2. temperatureunder cooling with ice
  3. washthe solution was washed with an aqueous sodium thiosulfate solution
  4. washwashed with an aqueous sodium hydrogen carbonate solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThen, the solvent was distilled off under reduced pressure
  7. customthe obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:2)

출처 및 근거

ORD 기록
ord-9d5b14b8d0d047caaa9609678c8d482c
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802713B2

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