37 results about "Hyocholic acid" patented technology

The invention discloses a method for extracting ursodesoxycholic acid. The method for extracting ursodesoxycholic acid comprises the steps of esterification, extraction, recrystallization, hydrolysis, secondary recrystallization and the like. According to the method for extracting ursodesoxycholic acid, porcine bile is taken as an extraction raw material, after bilirubin is extracted from the porcine bile, filtrate after hyodeoxycholic acid and hyocholicacid are extracted is collected, and separation is carried out to obtain the ursodesoxycholic acid; porcine bile raw material is available, so that preparation cost of the ursodesoxycholic acid is reduced; acetic anhydride is selected as an esterifying reagent in an extraction process, ursodesoxycholic acid and recrystallization refining conditions are determined, sodium hydroxide is adopted as an alkali catalyst, and total yield of the ursodesoxycholic acid is more than 15% by adopting the technologic process.

The invention discloses a method for removing hyocholic acid from chenodeoxycholic acid. The method comprises the steps of dissolving, residue removing, complexing, crystallizing, centrifugal separating, emulsifying, acidifying, drying, mother liquor treating and the like; high-boiling-point butyl acetate is utilized as solvent, volatilization of the solvent is reduced, a good separation effect is achieved by utilizing the unique dissolution property of butyl acetate to impurities, and the solvent belongs to a three-level low-toxicity dangerous chemical; the selective complexing characteristic of sec-butylamine to bile acid is utilized, and the hyocholic acid and other impurities can be separated to a higher degree. According to the separation and purification method, impurity removing is qualified in one time, the loss rate of the chenodeoxycholic acid is 5% or below and is greatly lower than the effective ingredient loss of 30% in a conventional crystallization method, the solvent can be recycled, three wastes are not generated, and the method is an environment-friendly, low-cost and efficient separation method.

The invention provides a method for preparing chenodeoxycholic acid and ursodesoxycholic acid by directly extracting and synthetizing from porcine bile paste or leftovers, comprising the following steps: using lower content (15-35%) porcine bile paste or leftovers and pre-processing it to remove off non-cholic acids impurities; removing off cholic acid impurities below the chenodeoxycholic acid in the thin layer chromatography by bromine oxidation or chromium oxidation; removing off cholic acid impurities above the chenodeoxycholic acid or the ursodesoxycholic acid in the thin layer chromatography by conventional reduction method; directly preparing the chenodeoxycholic acid or the ursodesoxycholic acid.

The invention discloses a 7-ketolithocholic acid intermediate and its preparation method and application. The invention uses hyocholic acid as a starting material, first performs esterification reaction, and then adds 2,2-dimethylpropane and hyocholic acid The unique 6,7 hydroxyl structure reacts to form parallel fork protection, and then selectively protects the 3-position hydroxyl group, and then uses the special space structure of hyocholic acid to selectively connect the leaving group to the 6-position to form 7-ketone Keystone cholic acid intermediate, 7-ketolithocholic acid intermediate unique 7-position exposed hydroxyl group, selective oxidation of 7-position hydroxyl group to form α-hydroxy ketone intermediate 6 with 6-position connecting leaving group, this type of hydroxyketone can be directly The hydroxyl group at the 6th position and the leaving group are removed simultaneously to form intermediate 7, and intermediate 7 can be deprotected by simple hydrolysis to obtain the target product 7-ketolithocholic acid. The 7-ketolithocholic acid prepared by the method of the present invention not only has high purity, but also has a simple process flow and no special purification method in the preparation process, which is suitable for industrial production.

The invention discloses a 7-ketolithocholic acid intermediate and its preparation process and application. The invention uses hyocholic acid as a starting material, and first performs an esterification reaction, and then a silane-type protecting group protects the 3-position with high selectivity. Hydroxyl, and then using the specific spatial structure of the 6 and 7 hydroxyl groups of hyocholic acid, the conventional protection method can selectively connect a strong leaving group at the 6-position to obtain the intermediate of 7-ketolithocholic acid, 7-ketolithocholic acid The acid intermediate is sequentially oxidized, removed, reduced, and hydrolyzed to remove the protecting group to obtain the target product 7-ketolithocholic acid. The 7-ketolithocholic acid prepared by the process of the present invention not only has high purity, but also has a simple process flow, greatly simplifies the synthesis route and saves industrialization costs.

The invention discloses a method for extracting chenodeoxycholic acid and allocholic acid from duck bile, and belongs to the technical field of biological engineering. The method comprises the following steps of (1) preparing of bile acid extracting liquid: obtaining duck bile, saponifying, cooling, adjusting a pH (potential of hydrogen) value to 7 to 8, adding a mixed solvent of ester and alkane, adjusting the pH value to 2 to 4, extracting, and discoloring, so as to obtain the bile acid extracting liquid; (2) preparing of bile acid magnesium salt: adjusting the pH value of the bile acid extracting liquid in step (1) to 4.5 to 5.5, dissolving the magnesium salt, adding into the bile acid extracting liquid, refluxing, cooling, and separating, so as to respectively obtain the magnesium allocholate and a chenodeoxycholic acid solution; refining and purifying the chenodeoxycholic acid solution, so as to obtain a finished product of henodeoxycholic acid; (3) extracting of the allocholic acid: adding water and carbonate into the prepared magnesium allocholate in step (2), heating and dissolving, separating solid from liquid, adjusting the pH value of a solution to 1 to 2, and separating solid from liquid, so as to obtain a finished product of the allocholic acid. The method has the advantages that the purities and extracting rates of the chenodeoxycholic acid and the allocholic acid are greatly improved, the operation is safe, and the method is suitable for industrialization.