Citric Acid → N-{4-[4-(Diethylcarbamoyl-phenyl-methyl)-piperazin-1-yl]-3-fluoro-phenyl}-2-pyridin-3-yl-benzamide citrate salt

Participants

Reaction Steps

To a 100 mL flask charged with absolute ethanol (25 mL) was added N-{4-[4-(diethylcarbamoyl-phenyl-methyl)-piperazin-1-yl]-3-fluoro-phenyl}-2-pyridin-3-yl-benzamide (495.4 mg, 0.87 mmol). Mild heating with a heat gun, sonication and addition of CH2Cl2 (4 mL) resulted in a homogeneous solution. Citric acid (171.1 mg) was then added in one portion and the resulting mixture was stirred until homogenous, then allowed to stand for 1 h. The solvents were removed with the rotary evaporator to yield an off-white foam. The foam was stirred over a 2:1 mixture of diethyl ether and ethyl acetate (60 mL) for 6 h. The resulting solids were collected on filter paper, washed with diethyl ether and dried under vacuum to yield the title compound as an off-white powder.

Provenance & Evidence