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Separation preparation method of bazedoxifene acetate impurity A

A bazedoxifene acetate and impurity technology, applied in the field of reference substance research, can solve the problems of low yield and difficulty in obtaining impurity A with a purity above 96%, and achieve the goal of optimizing chromatographic conditions, shortening separation time, and ensuring stability Effect

Inactive Publication Date: 2015-07-15
JIANGSU CAREFREE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the preparation method of impurity A is mainly chemical synthesis, but a large amount of by-products are easily produced during the synthesis process, and the yield is low, so it is difficult to obtain impurity A with a purity of 96% or more.

Method used

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  • Separation preparation method of bazedoxifene acetate impurity A
  • Separation preparation method of bazedoxifene acetate impurity A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In this example, 80% bazedoxifene was used as raw material, and 5 μm C 18 The bonded phase filler is a chromatographic column, and a solution containing 0.01M dipotassium hydrogen phosphate (PH8.3)-acetonitrile (40:60, volume ratio) is used as the eluting solvent. The specific process steps are as follows:

[0024] 1. Sample pretreatment

[0025] Add bazedoxifene to the eluting solvent to dissolve, add 3% hydrogen peroxide, let stand for half an hour, dilute the bazedoxifene solution to a concentration of 1 mg / ml with the eluting solvent, and filter through a 0.22 μm microporous membrane.

[0026] 2. Column handling

[0027] The preparative high-performance liquid chromatography column was selected as the stationary phase produced by Japan Sheshido Company as C 18 A preparative column (5 μm, 20×250 mm) was used to equilibrate the chromatographic column with an eluting system solution of about 5 times the column volume.

[0028] 3. Sample loading

[0029] The filtere...

Embodiment 2

[0039] In this example, 90% bazedoxifene was used as raw material, and 10 μmC 18 The bonded phase filler is a chromatographic column, and a solution containing 0.01M dipotassium hydrogen phosphate (PH8.3)-acetonitrile (35:65, volume ratio) is used as the eluting solvent. The specific process steps are as follows:

[0040] 1. Sample pretreatment

[0041] Add bazedoxifene to the elution solvent to dissolve, add 3% hydrogen peroxide, let it stand for 1 hour, dilute it with the elution solvent to a bazedoxifene solution with a concentration of 5 mg / ml, and filter through a 0.22 μm microporous membrane.

[0042] 2. Column handling

[0043] The preparative high-performance liquid chromatography column is selected as a self-packed preparative column, and the particle size of the filler is 10 μm C 8 Bonded phase filler (10μm, 75×250mm), equilibrate the chromatographic column with the elution system solution of about 10 times the column volume.

[0044] 3. Sample loading

[0045] T...

Embodiment 3

[0053] In this example, 85% bazedoxifene was used as raw material, and 10 μm C 18 The bonded phase filler is a chromatographic column, and a solution containing 0.01M dipotassium hydrogen phosphate (PH8.3)-acetonitrile (40:60, volume ratio) is used as the eluting solvent. The specific process steps are as follows:

[0054] 1. Sample pretreatment

[0055] Add bazedoxifene to the elution solvent to dissolve, add 3% hydrogen peroxide, let stand for half an hour, dilute the bazedoxifene solution to a concentration of 5 mg / ml with the elution solvent, and filter through a 0.45 μm microporous membrane.

[0056] 2. Column handling

[0057] The preparative high-performance liquid chromatography column is selected as a self-packed preparative column, and the particle size of the filler is 10 μm C 18 Bonded phase filler (10μm, 75×250mm), equilibrate the chromatographic column with the elution system solution of about 10 times the column volume.

[0058] 3. Sample loading

[0059] Th...

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Abstract

The invention relates to a method for preparing an impurity A having the purity of more than 97% from a bazedoxifene raw material, can be applied in research of reference substances and belongs to the field of medicine.

Description

technical field [0001] The invention relates to a preparation method for separating and obtaining impurity A with a purity greater than 97% from bazedoxifene raw materials, which can be applied to the research of reference substances. It belongs to the field of medicine. Background technique [0002] Bazedoxifene is a selective estrogen receptor modulator (SERM) with a new chemical structure. It can competitively inhibit the combination of estradiol and estrogen receptor ER, has estrogen agonist activity on bones, and can improve the bone density of the spine and hip, so it can significantly reduce the risk of vertebral fractures in postmenopausal women with osteoporosis. This product was developed by Wyeth-Ayerst Company of the United States (now Pfizer Company), and was approved by the European Union on April 27, 2009 for the treatment of postmenopausal osteoporosis. [0003] Bazedoxifene combined with estrogen prevents bone loss without stimulating the breasts or uterus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/12
CPCC07D209/12
Inventor 秦引林李敬芝
Owner JIANGSU CAREFREE PHARM CO LTD
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