ChemicalBook CAS DataBase List 3alpha-Hydroxy-7-oxo-5beta-cholanic Acid

3alpha-Hydroxy-7-oxo-5beta-cholanic Acid synthesis

6synthesis methods

Product Name:3alpha-Hydroxy-7-oxo-5beta-cholanic Acid
CAS Number:4651-67-6
Molecular formula:C24H38O4
Molecular Weight:390.56

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3alpha-Hydroxy-7-oxo-5beta-cholanic Acid

4651-67-6
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$39.00/500mg

Yield:4651-67-6 98.8%

Reaction Conditions:

with D-Glucose;sodium hydroxide in propane-1,2,3-triol at 30 - 35; pH=7 - 8; for 2 h;Enzymatic reaction;Solvent;

Steps:

1-3 Example 2

Add 300ml of water to a clean reaction flask, add 50.0g of compound I (purity: 99.1%) and 50.0ml of glycerol with stirring,Adjust pH=78 with 2N sodium hydroxide, after compound I is completely dissolved, adjust the reaction temperature to 3035 , add 120g glucose,10g 3α reductase, 22g glucose dehydrogenase, 1.5g coenzyme one, 1.5g coenzyme two.After stirring uniformly, adjust pH=7-8 with 2N sodium hydroxide solution, and react for 2 hours, until the content of compound I monitored by HPLC is 0.1%.After the reaction, the temperature of the system was raised to 70-80° C., and the temperature was kept stirring for 30-60 min.The filtrate was collected by suction filtration while hot, and the filter cake was again heated to 70-80° C. with 100 ml of water, kept stirring for 30-60 min, and the filtrate was combined after hot filtration.The filtrate was concentrated under reduced pressure at 50-60°C to remove glycerol, cooled to 0-10°C, and 2N hydrochloric acid was slowly added dropwise to adjust pH=2-3, a large amount of solid was precipitated, and the temperature was kept stirring for 30min-60min.Filter, rinse with a small amount of tap water, and dry the filter cake in a hot air circulating oven at 50°C until it is qualified.Dry weight: 49.4 g, LC purity: 98.1%.

References:

CN113968891,2022,A Location in patent:Paragraph 0024-0032

474-25-9 Synthesis