Hydrochloric Acid → HCID 21452755, compound

Participants

Reaction Steps

To a suspension of 10 grams of the 2-phenyl-3-acetyl-7-methylbenzofuran that was thus prepared in 40 milliliters of isopropanol was added 1.7 grams of paraformaldehyde, 4.6 grams of dimethylamine hyrochloride, and 4 milliliters of a saturated solution of hydrogen chloride in ethanol, and the mixture was heated at its boiling point for a period of 10 hours. The solvent was then evaporated from the mixture under vacuum and the residue was taken up in water, and the insoluble portions of the residue were extracted from the resulting solution with ethyl ether. The aqueous solution was then made alkaline by the addition thereto of a 5% aqueous solution of sodium hydroxide and the precipitated base was extracted therefrom by the addition of ethyl ether thereto. The ethyl ether extract was separated and dried over anhydrous sodium sulfate. A solution of hydrogen chloride in ethanol was then added to the dried ether extract, whereupon crystals of the hydrochloride of the compound named in the heading of this example precipitated therefrom. The crystals were separated by suction filtration and recrystallized from a mixture of ethanol and ethyl ether. In this manner, 13.2 grams of crystals of the hydrochloride, having a melting point of 145°-146.5° C, was obtained.

Provenance & Evidence