Obeticholic Acid Impurity 4 synthesis

Yield:61800-60-0 49.2 g

Reaction Conditions:

with hydrogenchloride for 2 h;Reflux;

Steps:

2.a a. Preparation of 3α, 6α, 7α trihydroxy-5β-cholanoic acid ethyl ester

In a 500ml three-necked flask, add 50g of porcine cholic acid, stir and dissolve with 300ml of absolute ethanol, add 0.5ml of concentrated hydrochloric acid, heat up and reflux for 2h, and the residual porcine cholic acid is 0.679% by sampling. Add 50 ml of sodium bicarbonate solution with a concentration of 1%, stir evenly, vacuum distillation, remove ethanol to obtain a large number of white crystals, filter, wash the filter cake with 200 ml of water, and dry it in a hot air circulating oven at 75 ° C for 8 hours to obtain 3α, 6α, 7α trihydroxy 49.2 g of -5β-cholanoic acid ethyl ester, the purity of which was detected by HPLC was 99.236%.

References:

CN114133421,2022,A Location in patent:Paragraph 0039; 0060-0063