Pyridine → HCID 86644433、化合物

HRID 2404509ノート

反応式

HRID 2404509 の反応式
[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].N1C=CC=CC=1.FC(F)(F)S([O-])(=O)=O.[F:39][C:40]([I+]C1C=CC=CC=1)([F:48])[C:41]([F:47])([F:46])[C:42]([F:45])([F:44])[F:43]>ClCCl>[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][C:40]([F:48])([F:39])[C:41]([F:47])([F:46])[C:42]([F:45])([F:44])[F:43])[CH:6]=1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 1049PyridineHCID 2760327(Heptafluoropropyl)(phenyl)iodanium trifluoromethanesulfonateHCID 178474353HCID 178474353、化合物

生成物 1

HCID 86644433HCID 86644433、化合物収率 3.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2.1 g of 5-acetylamino-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-hydroxypyrazole was dissolved in 60 mL of dichloromethane, and 0.51 g of pyridine was added. To the obtained solution, 3.0 g of (perfluoro-n-propyl)phenyliodonium trifluoromethanesulfonate was slowly added, followed by stirring at room temperature for 1 hour. The solvent was distilled off under reduced pressure, a saturated salt solution was added, extraction with ethyl acetate was carried out, the organic layer was dried over anhydrous sodium 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 0.10 g of 5-acetylamino-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-(1,1,2,2,3,3,3-heptafluoropropoxy)pyrazole.

後処理

  1. distillationThe solvent was distilled off under reduced pressure
  2. additiona saturated salt solution was added
  3. extractionextraction with ethyl acetate
  4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customthe obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:4)

出典と根拠

ORDレコード
ord-a20ff72843154df6814b04bed4d6eaad
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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