Tributylstannane → HCID 13508144, compound

Participants

Reaction Steps

To a solution of 2-(2-bromo-1,1,2-trifluoroethylthio)-4,5-bis(4-methoxyphenyl)imidazole (14.2 g., 0.03 mole) in 150 ml. toluene is added tri-n-butyltin hydride (9.0 g., 0.03 mole). The mixture is refluxed for four hours. Another 9.0 g. (0.03 mole) of tri-n-butyltin hydride is added and the mixture is refluxed overnight. The mixture is then added directly to a column of 2 lb. of silica gel (SilicAR® CC-7). Elution with toluene followed by toluene/ethyl acetate (95/5) gives 6.5 g. of crystalline product. A recrystallization from methylcyclohexane gives 5.6 g. of pure product, m.p. 143.5°-145°.

Provenance & Evidence