Formic Acid → 1-(4-Chlorobenzyl)-4-(2,4-dichlorocinnamyl)piperazine dihydrochloride

Participants

Reaction Conditions

Reaction Steps

N-(4-Chlorobenzyl)piperazine (4.2 g, 19.93 mmole) (which is prepared by the process as disclosed in Yoshiaki Ikeda et al., Yakugaku Zasshi, Vol. 89, 669-676, 1969) and 2,4-dichlorocinnamaldehyde (4.1 g, 20.39 mmole) (which is prepared by the process as disclosed in U.S. Pat. No. 3,094,561) are mixed and heated on an oil bath at 130° C. to melt them, and thereto is added dropwise formic acid (2.0 ml, 52.6 mmole), and the mixture is stirred under heating for 30 minutes. The reaction mixture is allowed to cool and is dissolved in ethanol (30 ml), and to the solution is added an ethanol solution (90 ml) of conc. hydrochloric acid (4.5 ml). The precipitated crystals are separated by filtration. The crystals are recrystallized from water-ethanol to give the title compound (3.8 g). The product shows the same physical properties as those of the compound prepared in Example 1-(1).

Provenance & Evidence