Process for preparing deoxycholic acid

Abstract

The invention discloses a process for preparing deoxycholic acid. The process comprises the following steps: (1) by taking chenodeoxycholic acid as a raw material, adding a proper solvent; (2) adding a reagent and a catalyst, and selectively generating a derivative together with 3alpha-hydroxyl; (3) adding a chiral inducer, an asymmetric synthesis catalyst, tertiary butanol or octyl pentanol, filling hydrogen and pressurizing, converting 7alpha-hydroxyl in the chenodeoxycholic acid into 7beta-hydroxyl through one step under radiation conditions, thereby generating a coarse product of chenodeoxycholic acid; (4) washing the coarse product of chenodeoxycholic acid, filtering and removing impurities; (5) selecting a corresponding solvent, and extracting to remove the unreacted chenodeoxycholic acid and other impurities; and (6) drying the chenodeoxycholic acid, and collecting and packaging to obtain a finished product. The process flow is simple, the equipment investment is low, fewer chemical reagents are used, the conversion rate is high, raw materials are fully utilized, the production efficiency is improved, the production cost and the energy consumption are greatly reduced, and the process is suitable for industrial production.

Description

technical field [0001] The invention relates to a process for preparing biochemicals, in particular to a process for preparing ursodeoxycholic acid. Background technique [0002] Ursodeoxycholic acid is one of the main active ingredients in bear bile. It is clinically used to dissolve gallstones, and it also has certain effects on toxic hepatitis, cholecystitis, primary sclerosing cholangitis, and primary cholestatic cirrhosis. treatment effect. [0003] Ursodeoxycholic acid can be extracted and isolated from bear bile, or synthesized by biosynthesis. [0004] Since 1955, Kanazawa proposed to use cholic acid as a raw material for the synthesis of ursodeoxycholic acid in 7 steps. In 1984, Giordano et al., UP4486352, Kimura et al. Oxycholic acid process has been improved, using alkali metal as reducing agent. [0005] Bharucha et al. in 1985, US4547271, Hatsutori et al. in 1994, and JP6002184 respectively proposed the process of preparing ursodeoxycholic acid by electrochem...

AI Technical Summary

Problems solved by technology

[0011] In principle, the aforementioned processes can produce ursodeoxycholic acid, but the 7-step or 2-step process first oxidizes chenodeoxycholic acid to 7-ketolithocholic acid, and then reduces it to ursodeoxycholic acid acid, there are many steps in the actual preparation process, therefore, there are still problems to be solved in the production, such as violent reaction, large energy consumption of solvent recovery, and low yield.