Hydrochloric Acid → HCID 21996630, compound

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Reaction Steps

3 g of the hydrochloride of the acetylene compound obtained in Example 1 are liberated with 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 residual oil is then taken up in 100 ml of ethyl acetate, after which 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 Celite and the filtrate is concentrated under vacuum. The residue obtained is taken up in the minimum amount of methanol in the presence of 50 ml of 2 N hydrochloric acid and is then successively extracted with dichloromethane, washed with 2N hydrochloric acid solution, with saturated sodium chloride solution, dried over magnesium sulphate and concentrated under vacuum in order to obtain 2 g of the expected hydrochloride; m.p.=266° C.

Provenance & Evidence