Ethanol → HCID 22013560, compound

Participants

Reaction Conditions

Reaction Steps

An autoclave is loaded with 7.0 g of 3-(5,6-dichloro-2-pyridyl)-4chloro 5trifluoromethyl-1-methyl-[1H]-pyrazole (Example H20), 100 ml of dry ethanol, 9.0 ml of triethylamine and 0.83 g of palladium bistriphenylphosphine dichloride (PdCl2(PPh3)2). 140 bar of carbon monoxide are forced in at 25° C. and the mixture is then kept at 120° C. for 15 hours. After cooling to 25° C., the mixture is concentrated and the residue is then absorbed onto silica gel from ethyl acetate. This silica gel is introduced onto a flash chromatography column and the column is then eluted with a mixture of n-hexane/ethyl acetate 7/1 (v/v). 4.51 g of the desired title compound are obtained as a yellow solid (58% of theory). TLC analysis: Rf value of the product (silica gel 60 F254, n-hexane/ethyl acetate 4/1 (v/v)): 0.19.

Provenance & Evidence