Ethanol → HCID 10905333, compound

Participants

Reaction Steps

A mixture of 4 g 1-(3-fluoro-5,6-dichloro-2-pyridyl)-3-methyl-4-trifluoromethylpyrimidin-2,6-dione (Example H4), 3.4 g triethylamine and 2 g dichloro-bis(triphenylphosphine)palladium in 50 ml ethanol is pressurized in an autoclave with carbon monoxide at 180 bar and the mixture heated for about 30 hours to 101° C., leading to a pressure build-up of max. 228 bar. The heating is then switched off, the reaction mixture left to stand at 22° C. over the weekend and filtered; the filtrate is then concentrated by evaporation in a vacuum, and the residue obtained is purified over a silica gel column (eluent: n-hexane/ethyl acetate 9/1). The desired title compound is obtained as a yellowish resin.

Provenance & Evidence