Reaction #521560

ord-d8c15482729c4ec7a030997491fe14e4

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperatureto cool
  2. 2
    Filtrationthe inorganic salt was filtered off
  3. 3
    Concentrationthe filtrate was concentrated in vacuo
  4. 4
    OtherAfter treatment with diisopropyl ether, the oily residue crystallized out
  5. 5
    OtherAfter drying

Procedure

13.45 g (1 mol) of 1-chloro-3,3-dimethyl-butan-2-one, 69 g (1 mol) of 1,2,4-triazole and 140 g (1 mol) of powdered potassium carbonate were heated under reflux in 500 ml of acetone for 6 hours, while stirring. Thereafter, the mixture was allowed to cool, the inorganic salt was filtered off and the filtrate was concentrated in vacuo. After treatment with diisopropyl ether, the oily residue crystallized out. After drying, 123.6 g (74% of theory) of 3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one of melting point 63°-65° C. were obtained.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04396624uspto-grants-1983_08