Hydrochloric Acid → HCID 70055746, compound

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Reaction Steps

3 g of the hydrochloride of the acetylenic compound obtained in Example 1 above are liberated by aqueous 10% sodium hydroxide solution. The oil obtained after extraction with diethyl ether is washed with saturated sodium chloride solution, dried over magnesium sulphate and concentrated under vacuum. The residue thus obtained is taken up in 100 ml of ethyl acetate, 5 ml of methanol are added, followed by 0.2 g of Pd/BaSO4 and the reaction mixture is hydrogenated at room temperature and at atmospheric pressure. The catalyst is separated out by filtration through silica, the filtrate is concentrated under vacuum and the residual oil is then chromatographed on a column of silica gel, eluent: 98/2 (v/v) dichloromethane/methanol. Concentration of the pure fractions gives the hydrochloride, which is recrystallized from ethyl acetate; Y=44%; m.p.=238° C.

Provenance & Evidence