Sulfuric Acid → HCID 86644424, 화합물

HRID 2404504노트

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HRID 2404504 반응식
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

참가 물질

5

반응물 2

HCID 1118Sulfuric AcidHCID 86644425HCID 86644425, 화합물

생성물 1

HCID 86644424HCID 86644424, 화합물수율 81.7%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-599c6ba4dd25462999c62f28c8fac04b
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802713B2

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