Sulfuric Acid → HCID 86644424、化合物

HRID 2404504ノート

反応式

HRID 2404504 の反応式
C([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]([O:24][C:25]([F:33])([F:32])[CH:26]([F:31])[C:27]([F:30])([F:29])[F:28])[CH:6]=1)(=O)C.S(=O)(=O)(O)O>C(O)C.O>[NH2:4][C:5]1[N:9]([C:10]2[CH:15]=[C:14]([S:16][CH2:17][C:18]([F:20])([F:21])[F:19])[C:13]([CH3:22])=[CH:12][C:11]=2[F:23])[N:8]=[C:7]([O:24][C:25]([F:32])([F:33])[CH:26]([F:31])[C:27]([F:28])([F:29])[F:30])[CH:6]=1

参加物

5

反応物 2

HCID 1118Sulfuric AcidHCID 86644425HCID 86644425、化合物

生成物 1

HCID 86644424HCID 86644424、化合物収率 81.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

1.2 g of 5-acetylamino-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-(1,1,2,3,3,3-hexafluoropropoxy)pyrazole was dissolved in 50 mL of ethanol, and an aqueous solution comprising 0.5 g of concentrated sulfuric acid in 2.0 mL of water was added, followed by reflux with heating for 6 hours. After cooling to room temperature, the solvent was distilled off under reduced pressure, and 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 0.9 g of 5-amino-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-(1,1,2,3,3,3-hexafluoropropoxy)pyrazole.

後処理

  1. additionwas added
  2. temperatureby reflux
  3. temperaturewith heating for 6 hours
  4. distillationthe solvent was distilled off under reduced pressure, and extraction with ethyl acetate
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. 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-599c6ba4dd25462999c62f28c8fac04b
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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