Hydrogen Peroxide → HCID 66679876, 화합물

HRID 1045118노트

반응식

HRID 1045118 반응식
[CH3:1][C:2]1[C:10]([S:11][CH3:12])=[C:9]([C:13]([F:16])([F:15])[F:14])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[OH:17]O>C(O)(=O)C>[CH3:1][C:2]1[C:10]([S:11]([CH3:12])=[O:17])=[C:9]([C:13]([F:14])([F:16])[F:15])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

참가 물질

4

반응물 2

HCID 784Hydrogen PeroxideHCID 574577672-Methyl-3-(methylthio)-4-(trifluoromethyl)benzoic acid

생성물 1

HCID 66679876HCID 66679876, 화합물수율 93.9%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
55 °C

실험 절차

1.00 g (4.00 mmol) of 2-methyl-3-(methylthio)-4-(trifluoromethyl)benzoic acid was introduced into 10 ml of glacial acetic acid. The mixture was heated to 50-60° C. At this temperature, 0.35 ml (35% strength, 4.00 mmol) of an aqueous hydrogen peroxide solution was added cautiously dropwise. The mixture was stirred at 60° C. for a number of hours until HPLC analysis no longer indicated any reactant. The reaction mixture was cooled and was worked up by washing with an aqueous 10% strength sodium hydrogensulfite solution. Following analytical verification of the absence of peroxides, the mixture was concentrated. The residue was taken up in water and then 1M hydrochloric acid was added. Extraction was carried out three times with ethyl acetate, and the combined organic phases were thereafter dried and freed from the solvents. 1.00 g of the clean product was isolated.

후처리

  1. temperatureThe reaction mixture was cooled
  2. washby washing with an aqueous 10% strength sodium hydrogensulfite solution
  3. concentrationthe mixture was concentrated
  4. addition1M hydrochloric acid was added
  5. extractionExtraction
  6. customthe combined organic phases were thereafter dried

출처 및 근거

ORD 기록
ord-441f292825734f37b982d343599a4d68
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08563779B2

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