Trifluoroacetic acid → HCID 54455838, compound

Participants

Reaction Steps

Trifluoroacetic acid (6 ml) is cooled to 5° C., and a solution of 0.8 g of N-[3-(5-t-butoxycarbonyl-2-pyridyl)acryloyl]-4-(4-diphenylmethyl-1-piperazinyl)butylamine (the free base of the product of Example 24) in 3 ml of dichloromethane is slowly added below 20° C. The mixture is stirred at room temperature overnight and concentrated. The residue is dissolved in 10 ml of water and washed with diethyl ether. The aqueous solution is adjusted to pH 5 with aqueous ammonium hydroxide and extracted with three 40-ml portions of ethyl acetate. The combined extracts are dried over magnesium sulfate and the solvent is distilled off. The residue is chromatographed on silica gel with chloroform-methanol (10:1) to give the title compound. m.p. 214°-216° C. (recrystallized from methanol)

Provenance & Evidence