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ChemicalBook CAS DataBase List Sodium deoxycholate
302-95-4

Sodium deoxycholate synthesis

5synthesis methods
Sodium deoxycholate can be prepared by that: 100g of industrial deoxycholic acid (purity 97%) in a 1000mL flask with mechanical stirring, reflux condenser and thermometer, 600mL of absolute ethanol, heating to 60 ℃ with stirring, adding 2g of activated carbon, and stirring for 2h, wherein the slightly turbid solution is obtained. Hot filtered and passed through a 0.45 μm microfiltration membrane. Slowly adding newly prepared sodium hydroxide ethanol solution (the mass concentration of sodium hydroxide is 6%) into the filtrate while stirring until the pH value of the reaction solution is 7.5, continuously stirring for 2h, concentrating under reduced pressure until the concentration of sodium deoxycholate is 25 wt%, cooling to room temperature, and continuously pulping for 5 h. Filtering, leaching the filter cake with absolute ethyl alcohol, drying at 85 ℃ to obtain 97.1g of white sodium deoxycholate powder, wherein the yield is 94.8%, the purity is 100%, the optical rotation is + 44.5%, the sodium content is 6.0%, the heavy metal content is less than or equal to 0.002%, and the arsenic content is less than or equal to 0.0002%.
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Yield:302-95-4 100%

Reaction Conditions:

with sodium hydroxide in methanol;lithium hydroxide monohydrate at 25;

Steps:

3.8; 6.8 Step 8:

Deoxycholic acid (1.30g, 3.3mmol, 1.0eq.) was added to a 100mL single-neck bottle,Add anhydrous methanol (20 mL) to dissolve, add an aqueous solution of sodium hydroxide (132.0 mg, 3.3 mmol, 1.0 eq.), stir at 25 ° C for 15-20 h, concentrate under reduced pressure to remove the solvent,Then, 2.6 ml of methanol and 20.8 ml of acetone were added to the reaction solution, and concentrated under reduced pressure.Drying gave sodium deoxycholate as a white solid (1.37 g, 100% yield).

References:

CN114716497,2022,A Location in patent:Paragraph 0139-0140; 0157-0158; 0180-0181; 0198-0199

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