m-Chloroperbenzoic acid → HCID 86644468、化合物

HRID 2404537ノート

反応式

HRID 2404537 の反応式
[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]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 86644467HCID 86644467、化合物

生成物 1

HCID 86644468HCID 86644468、化合物収率 77.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-9d5b14b8d0d047caaa9609678c8d482c
出典データセット
uspto-grants-2014_08
特許番号
US08802713B2

反応ノート

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