ChemicalBook CAS DataBase List LITHOCHOLIC ACID

LITHOCHOLIC ACID synthesis

8synthesis methods

Product Name:LITHOCHOLIC ACID
CAS Number:434-13-9
Molecular formula:C24H40O3
Molecular Weight:376.57

3α-Acetoxy-5β-cholan-24-oic acid methyl ester

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Yield:434-13-9 92%

Reaction Conditions:

with methanol;potassium carbonate in tetrahydrofuran at 70; for 24 h;Inert atmosphere;Concentration;

Steps:

1.7 7) Synthesis of compounds of formula (7)

Type (6) compound (200 mg, 0 . 46mmol) dissolved in methanol (10 ml) and tetrahydrofuran (2 ml) in the mixed solvent, adding anhydrous potassium carbonate (630 mg, 4 . 6mmol), nitrogen protection, heating to 70 °C, reaction 24 hours. TLC detection after the reaction is complete, the solvent is removed under reduced pressure, the addition of water (10 ml), diluted hydrochloric acid to adjust the pH of less than 7, dichloromethane is used for extraction (10 ml × 3), the combined organic phase, saturated salt water (20 ml × 3) washing, water-freeNa₂SO₄drying, concentration, silica gel column chromatography (DCM:MeOH=40:1) purification, to obtain white solid (7) compound (160 mg), yield 92%.

References:

CN106046093,2016,A Location in patent:Paragraph 0056; 0057