MOr-DESOXYCHOLIC ACID

The crude carbinol is acetylated and dehydrated by refluxing its solution in 1 1. of glacial acetic acid and 500 ml. of acetic anhydride for 1 hour. The solution is then concentrated to about 500 ml. by distillation. After cooling overnight, the crystalline 3,12-diacetoxy-5A or-cholanyldiphenylethylene is collected on a filter and washed with acetic acid. The yield is 95-105 g. (63.5-70.0%) of material melting at 154-157° (Note 5). This product is sufficiently pure to be used for the preparation of Mor-desoxycholic acid (p. 38) one crystallization from acetone gives white crystals which melt at 156-157.5° fully purified material melts at 159.5-160.5°. 

The crude diacetate is hydrolyzed by dissolving it in 350 ml. of 10% aqueous potassium hydroxide and refluxing the solution for 2 hours. The alkaline solution is diluted to about 700 ml., cooled, and filtered. The filtrate is poured into 300 ml. of 10% hydrochloric acid, and the Mor-desoxycholic acid is separated by filtration and dried. The crude product is dissolved in about 600 ml. of acetone and filtered, while hot, to remove small amounts of salt. On cooling, 25-30 g. (57-68%) of white crystals which melt at 209-211° is obtained in two crops (Note 5). This... 

The literature on methods of preparation is the same as that given for Mor-desoxycholic acid (p. 40). 

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See also in sourсe #XX -- [ , ]

See also in sourсe #XX -- [ , ]

See also in sourсe #XX -- [ , ]

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