Lithium Chloride → HCID 22390426, compound

Participants

Reaction Steps

0.76 g of dichlorobis(triphenylphosphine)palladium are added, under an inert atmosphere, to 3.6 g of 1-prop-2-ynylazepane (compound 4.1), 8 g of [4-(4,4-dimethylcyclohexyl)-3-chlorophenyl]trifluoromethanesulphonate (compound III.1), 0.103 g of copper iodide, 1.83 g of lithium chloride in 200 ml of triethylamine and 100 ml of pyridine. The reaction mixture is heated at reflux 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 95/5 (v/v) cyclohexane/ethyl acetate mixture. The residue obtained is taken up in diethyl ether and the hydrochloride is formed by bubbling hydrochloric acid through. After filtration, the residue obtained is recrystallized from toluene.

Provenance & Evidence