Obeticholic Acid Impurity 5 synthesis
- Product Name:Obeticholic Acid Impurity 5
- CAS Number:130081-08-2
- Molecular formula:C26H40O4
- Molecular Weight:416.6
Yield:130081-08-2 93.2 %
Reaction Conditions:
with sulfuric acid at 60;
Steps:
6.S1 S1: Esterification reaction between 3,7-diketocholanic acid and ethanol
Add the compound of formula (1) (1.94g, 5mmol) and absolute ethanol (40mL) to dissolve in a single-necked flask, then add concentrated sulfuric acid dropwise (0.1mL), reacted at 60°C for 5h, TLC detected that the raw materials were basically reacted completely, concentrated under reduced pressure to remove most of the methanol, added saturated NaHCO3 (20mL) and ethyl acetate (50mL) and stirred for 10min, separated, and washed the organic phase with saturated brine , dried over anhydrous sodium sulfate, concentrated under reduced pressure, and purified by column chromatography (PE/EA=20/1, v/v) to obtain ethyl 3,7-diketocholanoate (1.94 g, white solid), The molar yield was 93.2%.
References:
CN115819491,2023,A Location in patent:Paragraph 0164-0171
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