A kind of method utilizing hyodeoxycholic acid to prepare ursodeoxycholic 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., so as to reduce the production cost, reduce the safety production pressure, and reduce the consumption of coenzyme. 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 to 28 mL of concentrated sulfuric acid, dilute to 100 mL with water 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 allowing the mixture to stand for 10 min, a small amount of isopropanol was added to destroy the excess oxidant. The reaction mixture was filtered with celite, and concentrated under reduced pressure to remove the solvent to obtain 99.1 g of product R1 with a yield of 99.1%;
[0027] (2) 500mL reaction system, add 400mL 0.05M pH 6.8 PBS buffer to a 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 evenly and adjust the pH to 6.8, then add 15g 3α-HSDH, 25g 7β-hydroxylase, 10g GDH, kee...
Embodiment 2
[0029] Example 2 Using hyodeoxycholic acid to prepare ursodeoxycholic acid
[0030] (1) Add 22 g of chromium trioxide to 28 mL of concentrated sulfuric acid, and dilute to 100 mL with water to obtain Jones reagent. 50 g of hyodeoxycholic acid were dissolved in 1000 mL of ethyl acetate and treated with Jones reagent until a slight permanent orange color was obtained. After allowing the mixture to stand for 10 min, a small amount of isopropanol was added to destroy the excess oxidant. The reaction mixture was filtered with celite, and concentrated under reduced pressure to remove the solvent to obtain 48.8 g of intermediate R1 with a yield of 97.6%;
[0031] (2) 500 mL of reaction system, add 400 mL of 0.05M pH 7.0 PBS buffer to a 2L three-hole flask, then add 25 g of intermediate R1, 50 g of glucose, 40 mL of n-hexanol, 2.5 mL of Triton X-100, and 0.025 g of NAD + , put the three-hole flask in a 37°C constant temperature water bath, stir evenly and adjust the pH to 7.0, then ...
Embodiment 3
[0033] Example 3 Preparation of ursodeoxycholic acid using hyodeoxycholic acid
[0034] (1) Add 22 g of chromium trioxide to 28 mL of concentrated sulfuric acid, and dilute to 100 mL with water to obtain Jones reagent. 100 g of hyodeoxycholic acid were dissolved in 1000 mL of acetone and treated with Jones' reagent until a slight permanent orange color was obtained. After allowing the mixture to stand for 10 min, a small amount of isopropanol was added to destroy the excess oxidant. The reaction mixture was filtered with celite, and concentrated under reduced pressure to remove the solvent to obtain 98.2 g of product R1 with a yield of 98.2%;
[0035] (2) 500 mL of reaction system, add 400 mL of 0.05M pH 7.4 PBS buffer to a 2L three-hole flask, then add 75 g of intermediate R1, 230 g of glucose, 40 mL of n-hexanol, 2.5 mL of Triton X-100, and 0.3 g of NADPH. The flask was placed in a constant temperature water bath at 25°C, and the pH was adjusted to 7.4 after stirring evenly....
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