tert-Butyl methyl ether → HCID 21254021, compound

Participants

Reaction Steps

46.3 g (131 mmol) of Selectfluor™ were added to a solution of 40.2 g (131 mmol) of 3-(2,4-dichloro-5-methylphenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole in 0.5 l of acetonitrile. After the mixture had been stirred for 12 hours at room temperature, it was heated for a further hour at reflux temperature. Thereafter, three batches of 6.9 g (20 mmol) of Selectfluor™ were added to the reaction mixture, a little at a time, and the mixture was heated in each case for one hour at reflux temperature. The resulting mixture was subsequently treated with 0.5 l of methyl tert-butyl ether. The organic phase was washed with water, saturated aqueous sodium hydrogen carbonate solution and again with water, then dried over magnesium sulfate and finally concentrated. The crude product was purified by means of silica gel chromatography (eluent:hexane/ethyl acetate=9:1). Yield: 20.3 g.

Provenance & Evidence