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Preparation method of pitavastatin calcium oxide impurity

A technology for pitavastatin calcium and oxidized impurities is applied in the field of preparation of pitavastatin calcium oxidized impurities, which can solve the problems of low yield and the like, and achieve the effects of simple preparation method, improved quality control and medication safety.

Pending Publication Date: 2021-10-22
SHANGHAI JINGXIN BIOLOGICAL MEDICAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Use mCPBA as oxidant, ethyl acetate as solvent, react at 5-10°C, then warm to room temperature, react for 18-20h, but the yield is very low, mostly unreacted pitavastatin calcium salt

Method used

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  • Preparation method of pitavastatin calcium oxide impurity
  • Preparation method of pitavastatin calcium oxide impurity
  • Preparation method of pitavastatin calcium oxide impurity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Embodiment 1: Preparation of ImpK-1, ImpL-1, ImpO-1, ImpP-1

[0040] Take 10 grams of pitavastatin ester, dissolve it in 50 mL of organic solvent, stir at a certain temperature, add dropwise an organic solvent solution of 10% mass concentration of an oxidizing agent within 1 hour, and stir at room temperature for 4 hours, add sodium bicarbonate solution Quenched, the oil phase was separated and washed once more with sodium bicarbonate, spin-dried to obtain the crude product, and the pitavastatin ester was detected by LCMS. 494.35 (ImpO-1+ImpK-1) were 18.62%, 14.08%, 47.26%, respectively. ImpK-1, ImpL-1, ImpO-1, impP-1 were obtained by preparative chromatographic separation.

[0041] The specific results are shown in Table 1 below:

[0042] Table 1

[0043]

Embodiment 2

[0044] Embodiment 2: Preparation of ImpK-2, ImpL-2, ImpO-2, ImpP-2

[0045] Take 100 mg each of impK-1, impL-1, impO-1, and impP-1, add 1% alkaline aqueous solution, stir overnight at 20-25 degrees, wash the water phase with EA, and freeze-dry the water phase to obtain ImpK-2, ImpL-2, ImpO-2, ImpP-2.

[0046] The specific results of each program are shown in Table 2 below:

[0047] Table 2

[0048]

[0049] impK-2:

[0050] 1H NMR (400MHz, DMSO-d6) δ7.881 (d, J = 8.0Hz, 1H), 7.698-7.660 (m, 1H), 7.467-7.300 (m, 6H), 4.95 (s,) 4.20 (d, J=2.4Hz, 1H), 3.67(m, 1H), 3.250-3.239(m, 1H), 2.688-2.651(m, 2H), 2.012-1.965(m, 1H), 1.801-1.631(m, 1H) ), 1.378–1.056(m,5H), 1.108-1.031(m,1H)

[0051]13C NMR(101MHz,DMSO-d6)δ176.619,163.706,,161.272,162.629,146.896,145.620,132.740,132.429,132.352,131.885,131.805,129.806,128.862,127.785,126.230,125.879,125.573,116.153,115.941, 115.852, 115.640, 67.459, 66.509, 64.398, 53.387, 43.756, 40.833, 15.154, 11.563, 10.787; m / z: [M+H+]=438.2 ...

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Abstract

The invention relates to a preparation method of pitavastatin calcium oxide impurities, which comprises the following steps: by taking pitavastatin ester as a raw material, reacting with an oxidizing agent in an organic solvent to obtain an oxide of the pitavastatin ester, reacting with an inorganic alkali aqueous solution, and further hydrolyzing to obtain a salt of the oxide. The method can be used for qualitative and quantitative detection of impurities, and is beneficial to quality control and medication safety of pitavastatin.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical synthesis, and in particular relates to a preparation method of pitavastatin calcium oxidized impurities. Background technique [0002] In recent years, with the improvement of people's living standards and the continuous acceleration of the pace of work, the morbidity and mortality of cardiovascular diseases have shown an obvious upward trend. The incidence of hyperlipidemia among the middle-aged and elderly in western developed countries is as high as 60%. The prevalence of hyperlipidemia is more than 7%, and there are about 90 million hyperlipidemia patients. The general trend is that the north is larger than the south, and the city is larger than the countryside. Hyperlipidemia has become the number one killer threatening human health. The prevention and treatment of cardiovascular diseases in the early medical circles focused on the development of antihypertensive drugs, and later grad...

Claims

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Application Information

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IPC IPC(8): C07D405/04C07D215/60
CPCC07D405/04C07D215/60
Inventor 徐苗焕祝小平
Owner SHANGHAI JINGXIN BIOLOGICAL MEDICAL
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