HCID 131713059, compound → HCID 131713058, compound

Participants

Reaction Steps

Substance [2] (76.98 g, 145 mM) was dissolved in n-butanol (20 ml) and ethanol (300 ml). 5% Pd/C (15 g) was added thereto and catalytic hydrogenation was allowed to proceed for 3 hours. After removing the catalyst, the mother liquor was concentrated in vacuo. Diethyl ether (300 ml) was added to the residue, which was then extracted successively with 500 ml and 200 ml of 5% aqueous sodium bicarbonate. The extract was adjusted to pH 4 by adding 1 N HCl with ice cooling to precipitate the product continuously, which was extracted with ethyl acetate and washed twice with water. After drying with anhydrous sodium sulfate, the solution was concentrated in vacuo. The residue was solidified by adding ether-hexane. Recrystallization was effected with ethyl acetate-ether-hexane to obtain the substance [3] (60.33 g, yield: 94.2%).

Provenance & Evidence