Method for preparing ursodesoxycholic acid from hyodeoxycholic acid
A technology of hyodeoxycholic acid and ursodeoxycholic acid, which is applied in the field of biomedicine, can solve the problems of unfriendly environment, high safety risk, complicated process, etc., and achieve the goal of reducing production cost, reducing the pressure of safe production, and low coenzyme consumption Effect
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Embodiment 1
[0025] Example 1 Preparation of ursodeoxycholic acid using hyodeoxycholic acid
[0026] (1) Add 22 g of chromium trioxide into 28 mL of concentrated sulfuric acid and dilute with water to 100 mL to obtain Jones reagent; dissolve 100 g of hyodeoxycholic acid in 1000 mL of acetone and treat with Jones reagent until a slight permanent orange color is obtained. After the mixture was allowed to stand for 10 min, a small amount of isopropanol was added to destroy excess oxidizing agent. The reaction mixture was filtered with diatomaceous earth, concentrated under reduced pressure to remove the solvent, and obtained 99.1 g of product R1, with a yield of 99.1%;
[0027] (2) Reaction system 500mL, add 400mL 0.05M pH 6.8 PBS buffer solution to 2L three-hole flask, then add 50g intermediate R1, 120g glucose, 40mL n-hexanol, 2.5mL Triton X-100, 0.1g NADP + , put the three-hole flask in a constant temperature water bath at 35°C, stir well and then adjust the pH to 6.8, then add 15g 3α-HSD...
Embodiment 2
[0029] Example 2 Preparation of ursodeoxycholic acid using hyodeoxycholic acid
[0030] (1) Add 22 g of chromium trioxide into 28 mL of concentrated sulfuric acid and dilute to 100 mL with water to obtain Jones reagent. 50 g of hyodeoxycholic acid was dissolved in 1000 mL of ethyl acetate and treated with Jones reagent until a slight permanent orange color was obtained. After the mixture was allowed to stand for 10 min, a small amount of isopropanol was added to destroy excess oxidizing agent. The reaction mixture was filtered with diatomaceous earth, and concentrated under reduced pressure to remove the solvent to obtain 48.8g of intermediate R1 with a yield of 97.6%;
[0031] (2) Reaction system 500mL, add 400mL 0.05M pH 7.0 PBS buffer into 2L three-hole flask, then add 25g intermediate R1, 50g glucose, 40mL n-hexanol, 2.5mL Triton X-100, 0.025g NAD + , put the three-hole flask in a constant temperature water bath at 37°C, stir well and adjust the pH to 7.0, then add 7.5g ...
Embodiment 3
[0033] Example 3 Preparation of ursodeoxycholic acid by using hyodeoxycholic acid
[0034] (1) Add 22 g of chromium trioxide into 28 mL of concentrated sulfuric acid and dilute to 100 mL with water to obtain Jones reagent. 100 g of hyodeoxycholic acid was dissolved in 1000 mL of acetone and treated with Jones reagent until a slight permanent orange color was obtained. After the mixture was allowed to stand for 10 min, a small amount of isopropanol was added to destroy excess oxidizing agent. The reaction mixture was filtered with diatomaceous earth, and concentrated under reduced pressure to remove the solvent to obtain 98.2g of product R1 with a yield of 98.2%;
[0035] (2) With a reaction system of 500mL, add 400mL of 0.05M pH 7.4 PBS buffer to a 2L three-hole flask, then add 75g of intermediate R1, 230g of glucose, 40mL of n-hexanol, 2.5mL of Triton X-100, and 0.3g of NADPH. The well flask was placed in a constant temperature water bath at 25°C, stirred evenly, and adjusted...
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