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ChemicalBook CAS DataBase List EZM-K
191330-56-0

EZM-K synthesis

7synthesis methods
163222-33-1 Synthesis
Ezetimibe

163222-33-1
640 suppliers
$5.00/50mg

-

Yield:191330-56-0 75.7%

Reaction Conditions:

with potassium permanganate in tetrahydrofuran for 5 h;Reflux;Green chemistry;Solvent;Reagent/catalyst;

Steps:

6 Example 4 Preparation of Ketone Impurities
Ezetimibe (1 g, 2.44 mmol) was added to a 50 ml reaction flask, dissolved in 10 ml of tetrahydrofuran, and then potassium permanganate (0.58 g, 3.66 mmol) was added, and the mixture was stirred and heated at reflux for 5 hours. After the reaction of TLC was completed (petroleum ether:ethyl acetate=3:1, V/V), the solid was removed by filtration, and the filtrate was concentrated to dryness at a temperature of 40-50° C. to obtain a red-brown solid. To the solid was added 5 ml of isopropanol and 5 ml of water, stirred and dissolved by warming, and then the mixture was cooled to 0-5 DEG C and crystallized for 1 hour. Filter, filter cake with 2ml water, and drain. The filter cake was collected and dried at 60° C. to obtain 0.75 g of ketone impurities in a yield of 75.7%. 99.5% product purity by HPLC

References:

Hunan Fangsheng Pharmaceutical Co., Ltd.;Zhang Qinghua;Chen Bo;Xu Mi CN107474000, 2017, A Location in patent:Paragraph 0050; 0051

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