Hydrochloric Acid → HCID 66594577, compound

Participants

Reaction Steps

Compound 208-2 (0.360 g) was dissolved in a mixed solvent of tetrahydrofuran (4 ml) and water (1 ml), trifluoroacetic acid (1 ml) was added, and the mixture was stirred at room temperature for 4 hr. To the reaction mixture was added 1M aqueous sodium hydroxide solution, and the mixture was extracted with ethyl acetate, washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give a yellow oil. To a solution of the yellow oil in methylene chloride (5 ml) was added hydrogen chloride containing dioxane (4 mol/l, 5 ml), and the mixture was stirred at room temperature for 3 hr. The reaction mixture was concentrated, and the residue was washed with diethyl ether to give a white powder. The white powder was purified by HPLC, the obtained residue was converted to hydrochloride by adding hydrogen chloride containing ether (1 mol/l, 15 ml), and the precipitate was collected by filtration and dried to give the object product (110 mg) as a pale-brown powder.

Provenance & Evidence