Acetic Acid → HCID 59356394, compound

HRID 1670372Notes

Reaction equation

HRID 1670372 reaction equation
[CH2:1]([N:5]1[C:9]([S:10][CH3:11])=[CH:8][C:7]([C:12]([F:15])([F:14])[F:13])=[N:6]1)[CH2:2][CH2:3][CH3:4].OO.[OH2:18].C(O)(=[O:21])C>O.O.[O-][W]([O-])(=O)=O.[Na+].[Na+]>[CH2:1]([N:5]1[C:9]([S:10]([CH3:11])(=[O:21])=[O:18])=[CH:8][C:7]([C:12]([F:14])([F:13])[F:15])=[N:6]1)[CH2:2][CH2:3][CH3:4]

Participants

6

Reactant 4

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 962WaterHCID 59356407HCID 59356407, compound

Product 1

HCID 59356394HCID 59356394, compound

Reagents, catalysts & solvents 1

HCID 150191Sodium Tungstate DihydrateCatalyst

Procedure

4.40 g of Compound (15) was dissolved in 20 ml of acetic acid. While stirring, 6.36 g of a 30% hydrogen peroxide solution and 0.62 g of sodium tungstate dihydrate were added sequentially. The mixture was stirred at room temperature for 4 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 5.00 g of 1-butyl-5-methanesulfonyl-3-(trifluoromethyl)pyrazole (2-2).

Workup

  1. stirringThe mixture was stirred at room temperature for 4 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

Sources & evidence

ORD record
ord-8636b96f4422483fa21b276c841f138b
Source dataset
uspto-grants-2011_08
Patent number
US07994094B2

Reaction notes

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