Preparation method of tauro ursodesoxy cholic acid
A technology for tauroursodeoxycholic acid and ursodeoxycholic acid is applied in the field of preparing tauroursodeoxycholic acid, which can solve problems such as environmental pollution and achieve the effects of cheap materials, short reaction time and improved yield.
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[0047] Example 1 Preparation of Tauroursodeoxycholic Acid
[0048] 39.2 g (0.1 mol) of ursodeoxycholic acid was added to 100 ml of N,N-dimethylformamide, and the mixture was stirred to dissolve (the rotation speed was 150 rpm, stirring for 10 minutes). Cool down to 10°C, add 12.66g (0.11mol) of N-hydroxysuccinimide, stir to dissolve (rotate at 135rpm for 20 minutes), add 24.76g (0.12mol) of dicyclohexylcarbodiimide and 4-di 0.12 g (0.001 mol) of methylaminopyridine, after all the materials were added, the reaction was stirred at 12° C. for 2.5 hours at a speed of 135 rpm, and the content of ursodeoxycholic acid detected by HPLC was less than 0.1%, and the reaction was stopped. In addition, 12 g (0.12 mol) of taurine was dissolved in 500 ml of sodium hydroxide aqueous solution (containing 4.8 g of sodium hydroxide, 0.12 mol) to obtain an aqueous solution of taurine sodium salt. The above dimethylformamide solution was added to the taurine sodium salt aqueous solution, and 34ml (0...
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[0049] Example 2 Preparation of Tauroursodeoxycholic Acid
[0050] 39.2 g (0.1 mol) of ursodeoxycholic acid was added to 100 ml of tetrahydrofuran, and stirred to dissolve (rotating speed 150 rpm, stirring for 10 minutes). Cool down to 0°C, add 12.66g (0.11mol) of N-hydroxyphthalimide, stir to dissolve (rotate at 150rpm and stir for 20 minutes), add 15.14g (0.12mol) of diisopropylcarbodiimide and 0.12 g (0.001 mol) of 4-dimethylaminopyridine. After all the materials were added, the reaction was carried out at 8°C for 20 minutes. The content of ursodeoxycholic acid detected by HPLC was less than 0.1%, and the reaction was stopped. In addition, 12 g (0.12 mol) of taurine was dissolved in 500 ml of sodium hydroxide aqueous solution (containing 4.8 g of sodium hydroxide, 0.12 mol) to obtain an aqueous solution of taurine sodium salt. The above tetrahydrofuran solution was added to the taurine sodium salt aqueous solution, and 34 ml (0.24 mol) of triethylamine was added dropwise. Aft...
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[0051] Example 3 Preparation of Tauroursodeoxycholic Acid
[0052] 39.2 g (0.1 mol) of ursodeoxycholic acid was added to 100 ml of dimethyl sulfoxide, and the mixture was stirred to dissolve (the rotating speed was 150 rpm and the stirring was for 10 minutes). Cool down to 10°C, add 12.66g (0.11mol) of N-hydroxysuccinimide, stir to dissolve (rotation speed is 150rpm, stir 10), add 1-ethyl-3-(3-dimethylaminopropyl) carbon two 18.62g (0.12mol) of imine and 012g (0.001mol) of 4-dimethylaminopyridine. After all the materials were added, the reaction was stirred at 8°C for 20min at a speed of 150rpm. The content of ursodeoxycholic acid detected by HPLC was less than 0.1% , Stop the reaction. In addition, 12 g (0.12 mol) of taurine was dissolved in 500 ml of sodium hydroxide aqueous solution (containing 4.8 g of sodium hydroxide, 0.12 mol) to obtain an aqueous solution of taurine sodium salt. The above methylene chloride solution was added to the taurine sodium salt aqueous solution,...
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