Hydrochloric Acid → HCID 23045030, compound

Participants

Reaction Steps

To a mixture of thiophene-2-carboxylic acid (0.4 g), 1-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride (1.1 g), triethylamine (1.2 g) and dimethylformamide (20 ml) is added dropwise, while stirring, diethyl cyanophosphonate (1.2 ml), followed by stirring for one hour. To the reaction mixture are added water (100 ml) and ethyl acetate (100 ml), followed by extraction. The extract is washed with water, dried and concentrated under reduced pressure. The residue is purified by means of a silica gel column chromatography (hexane:acetone=2:1) to give an oily product, which is led to its hydrochloride in a mixture of ethyl acetate - ethyl ether to yield 1-(2-thenoyl)-4(3,4,5-trimethoxybenzyl)piperazine hydrochloride (0.65 g) as colorless needles, m.p. 205°-209° C. (decomp.).

Provenance & Evidence