Methyl Bromide → HCID 11214802, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of the potassium salt of 1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-trifluoromethylsulfinyl-5-(ethoxyacetamido)pyrazole, prepared in Step 1 above, (18.9 g, assay=75.6%, 0.026 mol) in 56.8 g of acetonitrile, a solution of methyl bromide in acetonitrile (86.5 g, conc=28%, 0.255 mol) was added. The mixture was stirred during 6 hours at 60° C. and then concentrated to dryness. The residue was solubilized in a mixture of toluene (100 g) and water (100 g). The organic layer was washed with 100 g of water and concentrated to a 38% solution, heated to 80° C. and product was recrystallized in a 40/60 toluene/n-heptane solution to afford 10.3 g of a white solid (yield=64%, assay=85%).

Provenance & Evidence