反应详情

In one embodiment in Step 5, E/Z-3α-hydroxy-6-ethylidene-7-keto-5β-cholan-24-oic acid (5A), water, NaOH solution (e.g. 50% wt.), and Pd/C are mixed at about 5 bar of H2 gas and at a temperature at about 100° C. to about 105° C. until H2 uptake has ceased. The reaction mixture is cooled to about 40° C. to about 50° C. and Pd/C is filtered off. Then n-butyl acetate and HCl are added to the solution containing compound 6. In one embodiment, the aqueous phase is separated and discarded. The organic phase containing compound 6 is treated with activated carbon. The carbon is filtered off and the filtrate is moved to another reactor where it is reduced down by distillation, and then the suspension is cooled to about 5° C. to about 20° C. In one embodiment, compound 6 is isolated via filtration and the filtrate is dried on the pressure filter under vacuum at about 80° C.

1. temperatureThe reaction mixture is cooled to about 40° C. to about 50° C.
2. filtrationPd/C is filtered off
3. additionThen n-butyl acetate and HCl are added to the solution
4. additioncontaining compound 6
5. customIn one embodiment, the aqueous phase is separated
6. additionThe organic phase containing compound 6
7. additionis treated with activated carbon
8. filtrationThe carbon is filtered off
9. customthe filtrate is moved to another reactor
10. distillationwhere it is reduced down by distillation
11. temperaturethe suspension is cooled to about 5° C. to about 20° C