Hydrochloric Acid → 3-(3-Fluoro-4-methoxyphenyl)prop-2-enoic acid

Participants

Reaction Steps

A mixture of 3-fluoro-anisaldehyde (1.5 g) and malonic acid (2.08 g) in 5 ml pyridine was warmed until clear solution was obtained. To this mixture piperidine (0.4 ml) was added and then the content of the flask was heated at 80° C. for one (1) hour. It was further refluxed for 3 hours. At the end of this period the mixture was poured into 50 ml of cold water. It was then acidified by adding 5 ml of concentrated hydrochloric acid. Upon addition of acid, the solid separated, which was filtered and washed with cold water. The material was dried. Yield=1.7 g. The crude material was crystallized from a mixture of tetrahydrofuran and water. m.p. 227°-230° C.

Provenance & Evidence