Hydrochloric Acid → HCID 54133978, compound

Participants

Reaction Steps

14 ml of dihydropyran was added dropwise to a mixture of 17.8 g of 4-methoxycinnamic acid, 0.34 g of 4-toluene sulphonic acid and 100 ml of diethyl ether under a nitrogen atmosphere. After one hour stirring the solution became transparent. 150 ml of ether was added and it was extracted with 200 ml of 5% of sodium hydroxide solution and evaporated using a rotary evaporator. The residue was mixed with 50 ml of ethanol and a solution of 8 g of KOH in 50 ml of water and was refluxed for 1 hour upon which a transparent solution was obtained. It was cooled with 150 g of crushed ice. Then 50 ml of HCl (2.5 N) was added dropwise to the solution until pH=4 upon which a solid precipitated. It was filtered off and washed with water. The product was dried in a dessicator over silica. 19.59 g (yield 79%) of a white solid was obtained.

Provenance & Evidence