1H-1,2,4-Triazole → HCID 13021647, compound

HRID 845564Notes

Reaction equation

HRID 845564 reaction equation
Br[CH:2]([F:9])[C:3](=[O:8])[C:4]([CH3:7])([CH3:6])[CH3:5].[NH:10]1[CH:14]=[N:13][CH:12]=[N:11]1.C(=O)([O-])[O-].[K+].[K+]>CC(CC)=O>[F:9][CH:2]([N:10]1[CH:14]=[N:13][CH:12]=[N:11]1)[C:3](=[O:8])[C:4]([CH3:7])([CH3:6])[CH3:5]

Participants

5

Reactant 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 13021645HCID 13021645, compound

Product 1

HCID 13021647HCID 13021647, compoundYield 84.4%

Reagents, catalysts & solvents 1

HCID 6569Methyl Ethyl KetoneSolvent

Procedure

63.0 g of 1-bromo-1-fluoro-3,3-dimethyl-2-butanone are added slowly to a mixture of 23.0 g of 1,2,4-triazole and 44.2 g of potassium carbonate in 280 ml of ethyl methyl ketone. The reaction mixture is stirred for 18 hours at 45°-50° C. and is then filtered and evaporated. The residue is taken up in methylene chloride and washed with water. Drying and evaporating the organic phase gives 50.0 g of 1-fluoro-1-(1H-1,2,4-triazol-1-yl)-3,3-dimethyl-2-butanone, melting point 54°-55° C.

Workup

  1. filtrationis then filtered
  2. customevaporated
  3. washwashed with water
  4. customDrying
  5. customevaporating the organic phase

Sources & evidence

ORD record
ord-a888a5ac4ab340feadd074048f99d1b7
Source dataset
uspto-grants-1988_07
Patent number
US04758670

Reaction notes

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