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ChemicalBook CAS DataBase List Cholan-24-oic acid,3-hydroxy-7-oxo-, phenylmethyl ester,(3α,5β)-

Cholan-24-oic acid,3-hydroxy-7-oxo-, phenylmethyl ester,(3α,5β)- synthesis

3synthesis methods
-

Yield:1352328-64-3 98.1%

Reaction Conditions:

Stage #1: 7-Ketolithocholic acidwith potassium carbonate in tetrahydrofuran; for 1 h;Reflux;
Stage #2: benzyl bromide in tetrahydrofuran; for 12 h;

Steps:

4.a a) Preparation of benzyl 3α-hydroxy-7-oxo-5β-cholanoic acid ester

3α-Hydroxy-7-oxo-5β-cholanoic acid (39.0 g, 100 mmol),Potassium carbonate (15.2g110mmol)Soluble in 200ml tetrahydrofuran,The mixture was warmed to reflux with stirring and the reaction was incubated for 1 hour.Benzyl bromide (18.0 g, 105 mmol) was slowly added dropwise.After dropping,Incubation reaction for 12 hours.Cool to room temperature, suction filtration, concentration of the filtrate,3α-Hydroxy-7-oxo-5β-cholanoic acid benzyl ester(471.6 g, yield 98.1%).

References:

CN107383139,2017,A Location in patent:Paragraph 0029