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Analysis method of empagliflozin
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A technology of empagliflozin and analysis method, applied in the field of analysis of empagliflozin, can solve problems such as the analysis method is not completely satisfactory, and achieve the effect of improving product quality and improving purity
Pending Publication Date: 2021-03-26
BEIJING KANG LISHENG PHARMA TECH DEV
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Patent CN201510160852.1 uses methyl ethyl ketone / water (1:1) to prepare Empagliflozin B crystal form, and the sample purity is improved to a certain extent. These existing patents reduce the content of related substances, but their analysis methods are still not fully satisfied. people are satisfied
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Embodiment 1
[0089]Example 1: Preparation of Engel Column (1)
[0090]
[0091]140 ml of dichloromethane, 140 mL acetonitrile, 70.0 g of compound 2 and 49.0 g of triethylsilane were sequentially added to a 1000 ml reaction bottle, and the bottle was lowered to ≤ -10 ° C, stirred and stirred, and 40.0 g of a borontrifluoride is added over the bottle. EtOAc. After Jianshi, the temperature was continued ≤ -10 ° C for 3 h, and the reaction was stopped. The solution of 30% sodiumcarbonate solution was added to a 1000 ml reaction bottle, and the solution pH was approximately 7, and the organic solvent was evaporated under reduced pressure, 200.0 ml of purified water and 200.0 ml of ethyl acetate, stirred, and water in the bottle containing the residue. EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc To dry, 140.0 ml of dichloromethane was stirred and reflux, crystalline, filtered, dried, and obtained 58.0 g Engel column (1) raw material crude product, yield was 88.4%, HPLC purity 98.77%.
[0099]6g Engel Jack Intermediate 2, added to the mixed solvent of water and THF (1: 1), add 4 mL of methylsulfonic acid, and stirred at room temperature for 8 h, TLC detection. After the reaction, 100 ml of ethyl acetate, separation, 100 ml of ethyl acetate was washed with EtOAc, and then the organic phase was washed with saturated aqueous sodium hydrogencarbonate, brine, sodium sodium sulfate, dry dry, silica gelcolumn chromatography, flow Phase ethanol: chloroform 1: 9 elution, get 1.9G light yellow solid,
[0100]The pale yellow solid 0.9 g, acetonitrile 50 ml, 12.5 ml of water was added, and 5 mg of sodium borohydride was added at room temperature for 30 min. After the reaction was completed, the acetonitrile was removed, and ethyl acetate (20 mL) was added twice, the combined organic phase concentrated, silica gel ...
Embodiment 3
[0111]Example 3: Preparation of CDM
[0112]10 mL of methanol and 5.0 g Engel column were sequentially added to 50 ml of reaction flask, stirred, stirred with 20 mL of dichloromethane, stir, precipitate, filtered, filter cake to dryness, stand for 24 hours, 4.3 g of C crystal Engel colleagues, yield of 86.0%, purity 99.91%.
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Abstract
The invention relates to an analysis method of empagliflozin, wherein the method comprises the steps: precisely weighing a proper amount of any one of empagliflozin products, adding methanol to dissolve, and diluting to prepare a test solution; and analyzing the test solution by adopting an HPLC method. The empagliflozin product comprises an empagliflozin raw material crude product, an empagliflozin raw material, an empagliflozin raw materialdrug, an empagliflozin reference substance, an empagliflozin standard substance, an empagliflozin crystal form, an empagliflozin C crystal form, an empagliflozin raw material intermediate, an empagliflozin-containing composition, an empagliflozin preparation, an empagliflozin tablet and an empagliflozin sustained-release tablet.
Description
Technical field[0001]The present invention relates to the field of pharmaceutical analysis, and in particular to an Engel-ranginganalysis method.Background technique[0002]Engel Jack, English Name: Empagliflozin, Engel Jack is R & D to Burlinger Yongham Company and Li Jing Company. The trade name is Jardiance. On March 21, 2014, the European Pharmaceutical Authority (EMA) Pharmaceutical Commission recommended to approve the sodium-dependent glucose copper SGLT (especially SGLT2) inhibitor Engel rings to treat adult type II diabetes patients.[0003][0004]Engel is a polymorphic compound, Engel rock crystal form and its preparation method are disclosed in WO2006 / 117359, and China's 2011 patented is CN200680011591.6, patent CN200680011591.6 with solvent C1-4-alkanol, Water, ethyl acetate, acetonitrile, acetone, diethyl ether, and two or more solvents, resulting in Engel Lexa A crystalline form, during its preparation process, there is some relevant substances in the final substance. Pa...
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