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Acetic Acid → 5-Methanesulfonyl-1-methyl-3-(trifluoromethyl)pyrazole

HRID 1670369
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HRID 1670369 반응식
[CH3:1][N:2]1[C:6]([S:7][CH3:8])=[CH:5][C:4]([C:9]([F:12])([F:11])[F:10])=[N:3]1.OO.[OH2:15].C(O)(=[O:18])C>O.O.[O-][W]([O-])(=O)=O.[Na+].[Na+]>[CH3:8][S:7]([C:6]1[N:2]([CH3:1])[N:3]=[C:4]([C:9]([F:12])([F:11])[F:10])[CH:5]=1)(=[O:18])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 962WaterHCID 593563841-Methyl-5-methylthio-3-(trifluoromethyl)pyrazole

생성물 1

HCID 593563985-Methanesulfonyl-1-methyl-3-(trifluoromethyl)pyrazole

시약·촉매·용매 1

HCID 150191Sodium Tungstate Dihydrate촉매

실험 절차

0.25 g of Compounds (14) was dissolved in 20 ml of acetic acid. While stirring, 0.44 g of 30% hydrogen peroxide solution, and 0.04 g of sodium tungstate dihydrate were added sequentially. The mixture was stirred at room temperature for 12 hours, then poured into water, and extracted with ethyl acetate. The organic layer was washed with saturated sodium hydrogencarbonate, dried over magnesium sulfate, and then filtered. The filtrate was concentrated under reduced pressure to produce 0.29 g of 5-methanesulfonyl-1-methyl-3-(trifluoromethyl)pyrazole (2-1).

후처리

  1. stirringThe mixture was stirred at room temperature for 12 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated sodium hydrogencarbonate
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-42b6c6a74d7c4e57b1b24da8832acf29
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07994094B2

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