Hydrochloric Acid → HCID 20533589, compound

Participants

Reaction Steps

A Grignard solution, freshly prepared from 4 g of magnesium and 20 g of ethyl bromide in 20 ml of tetrahydrofuran, is slowly added at 0° C. to a solution of 8 g of methylacetylene in 100 ml of tetrahydrofuran, and the mixture is stirred under argon for 15 minutes. There is then added dropwise to this mixture at 0° to 5° C. a solution of 27 g of o-phenoxybenzaldehyde in 100 ml of tetrahydrofuran. After being stirred for 14 hours at room temperature, the reaction mixture is cooled to 0° C. with 50 g of ice; 25 ml of conc. hydrochloric acid is subsequently slowly added, and extraction is performed with ether. The ether extract is washed twice with water and twice with saturated sodium chloride solution; it is then dried over sodium sulfate, filtered, and concentrated by evaporation. The product is chromatographed through silica gel with ethyl acetate/hexane (1:1) as the eluant. There is thus obtained the compound of the formula ##STR5## having a refractive index of nD20 =1.5898.

Provenance & Evidence