Lithium Chloride → HCID 70115228, compound

Participants

Reaction Steps

1.42 g of dichlorobis(triphenylphosphine)palladium are added, under an inert atmosphere, to 8.03 g of cyclohexylethylprop-2-ynylamine (compound 4.1), 15 g of [4-(4,4-dimethylcyclohexyl)-2-chlorophenyl] trifluoromethanesulphonate (compound 111.1), 0.19 g of copper iodide, 3.4 g of lithium chloride in 200 ml of triethylamine and 100 ml of pyridine. The reaction mixture is refluxed for 12 hours. The solvents are evaporated off under reduced pressure and the residue obtained is purified by chromatography on a column of silica gel, eluting with a cyclohexane/ethyl acetate mixture varying from 95/5 to 90/10 (v/v). The residue obtained is taken up in diethyl ether. The hydrochloride is separated out by filtration and hydrogen chloride is then bubbled through. The residue obtained is recrystallized from ethyl acetate.

Provenance & Evidence