Abstract
The comminuted air-dry raw material (i00.0 g) was loaded into a Soxhlet apparatus and was extracted with petroleum ether for 2 h to eliminated impurities. The cartridge with the plant material was dried in the air and was again charged into the Soxhlet apparatus and was extracted with methanol. The methanolic extract was cooled, whereupon an amorphous greyishgreen precipitate deposited, which was separated off by filtration. Then the methanol was distilled off from the filtrate on the water bath and the residue was combined with the residue on the filter. The dried greyish-green amorphous powder gave positive Liebermann-Burchard and Salkowsky reactions and the reaction with chlorosulfonic acid. For purification, the substance was repeatedly treated with ether, and the extract was passed through a column containing 50.0 g of activated carbon. The ether was distilled off on the water bath and the residue was recrystallized from acetone. After further recrystallization, the substance had mp 282-283°C, [~]~0 +63.2 ° (c 1.0; chloroform).
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