Method for producing ursodesoxycholic acid from 86% of chenodeoxycholic acid
A technology of chenodeoxycholic acid and ursodeoxycholic acid, which is applied in the field of treatment of gallstones and the preparation of liver-protecting drugs, can solve the problems of scarcity of bear bile medicinal materials and low cost, and achieve low cost and low production cost , The effect of easy-to-obtain raw material sources
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[0028] Example 1
[0029] Take 10 kg of chenodeoxycholic acid with a content of 86%, add 10 times the amount of methanol to dissolve at 60°C for 5 hours, then lower the temperature to 10°C after dissolution, then add 10% bromine solution and stir at 8°C for 8 hours. Then increase the temperature to 60℃ and add 30kg of sodium carbonate, then add 500kg of water to produce precipitation, filter, and vacuum-dry the crystals at 80℃ for 8 hours to obtain 7-ketone; take 10kg of 7-ketone, then add 30kg of tert-butanol at the temperature Dissolve at 60°C for 2 hours, then add 5 kg of sodium metal, stir at 90°C for 2 hours, then stop stirring, filter, and dry the crystals in vacuum at 80°C. Take 10kg of the above dried product, then add 30kg ethyl acetate, then add 2kg of triethylamine to dissolve at 60℃, and stir for 2 hours, then adjust the pH to about 2.5 with HCL, filter, crystallize, and vacuum dry at 80℃ to obtain the purity UDCA above 98.5%.
Example Embodiment
[0030] Example 2
[0031] Take 5kg of chenodeoxycholic acid with a content of 86% as raw material, add 6 times the amount of methanol, heat to 60°C, and dissolve for 7 hours;
[0032] Lower the temperature of the above-dissolved solution to 5°C, then add 7% bromine solution, and react at 5°C for 10 hours;
[0033] The above-mentioned reaction solution is heated to 50°C, 20kg of sodium carbonate is added, 400kg of water is added to filter, the filtrate is discarded, and the crystals are vacuum dried at 70°C to obtain 7-ketone;
[0034] Take 6kg of the 7-ketone mentioned above, add 20kg of tert-butanol, heat up to 50°C to dissolve, add 3kg of metallic sodium, stir at 70°C for 3 hours, then stop stirring, filter, and dry the crystals in vacuum at 70°C;
[0035] Take 6kg of the above crystalline product, add 20kg ethyl acetate, then add 0.5kg triethylamine to dissolve at 40℃, and stir for 3 hours, then adjust the pH to about 2.5 with HCl, filter, discard the filtrate, and dry the crys...
Example Embodiment
[0036] Example 3
[0037] Take 20kg of chenodeoxycholic acid with a content of 86% as raw material, add 15 times the amount of methanol, heat at 70°C, and dissolve for 3 hours;
[0038] Lower the temperature of the above-dissolved solution to 10°C, then add 12% bromine solution, and react at 10°C for 6 hours;
[0039] The above-mentioned reacted solution is heated to 60°C again, then 40kg of sodium carbonate is added, 650kg of water is added to filter, the filtrate is discarded, and the crystals are vacuum dried at 90°C to obtain 7-ketone;
[0040] Take 12kg of the above 7-ketone, add 40kg of tert-butanol, heat to 70°C to dissolve, add 8kg of metallic sodium, stir at 100°C for 1 hour, then stop stirring, filter, and dry the crystals in vacuum at 100°C;
[0041] Take 12kg of the above crystalline product, add 50kg ethyl acetate, and then add 3kg triethylamine to dissolve at 75°C, and stir for 1 hour, then adjust the pH to about 2.5 with HCl, filter, discard the filtrate, and dry th...
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