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A kind of preparation method of alogliptin benzoate polymorph crystal

A technology of benzoic acid and polymorphism, which is applied in the field of preparation of polymorphic crystals of alogliptin benzoate, can solve the problems of insufficient purity and inconsistent crystal forms, and achieve the effects of high purity, easy control, and convenient industrial production

Active Publication Date: 2016-01-20
JIANGSU DEYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] The technical problem to be solved by the present invention is aimed at the deficiencies in the prior art, and a method for preparing alogliptin benzoate polymorphic crystals is provided to solve problems such as inconsistent crystal forms and insufficient purity of products in the existing technology, and has the advantages of Advantages of high efficiency, energy saving and low cost

Method used

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  • A kind of preparation method of alogliptin benzoate polymorph crystal
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Embodiment 1

[0040] A preparation method of alogliptin benzoate polymorphic crystal, the steps are:

[0041] (1) Add methanol to the reaction kettle and stir, then add the synthetic alogliptin benzoate crude product, heat and reflux for 15 minutes, press filter into the crystallization kettle of the fine drying bag and stir, and then press into the crystallization kettle Butyl ether, naturally cooled to room temperature, stirred and crystallized for 3 hours; the consumption of described methanol was equivalent to 4.5 times of the crude product quality of alogliptin benzoate; the consumption of described methyl tert-butyl ether was equivalent to benzoic acid 2.5 times the mass of alogliptin crude product;

[0042] (2) Centrifuge, wash the obtained solid with methanol, and dry at 45° C. to obtain alogliptin benzoate polymorphic crystal product with a yield of 69.1% and a purity of 99.99% by HPLC.

Embodiment 2

[0044] A preparation method of alogliptin benzoate polymorphic crystal, the steps are:

[0045] (1) Add methanol into the reaction kettle and stir, then add the synthetic alogliptin benzoate crude product, heat and reflux for 30 minutes, press filter into the crystallization kettle of the fine drying bag and stir, and then press into the crystallization kettle Butyl ether, naturally cooled to room temperature, stirred and crystallized for 4 hours; the consumption of described methanol was equivalent to 7 times of the quality of alogliptin benzoate crude product; the consumption of described methyl tert-butyl ether was equivalent to benzoic acid 7 times the mass of alogliptin crude product;

[0046] (2) Centrifuge, wash the obtained solid with methanol, and dry it with blower at 55°C to obtain alogliptin benzoate polymorphic crystal product with a yield of 74.7% and a purity of 99.98% by HPLC.

Embodiment 3

[0048] A preparation method of alogliptin benzoate polymorphic crystal, the steps are:

[0049] (1) Add methanol into the reaction kettle and stir, then add the synthetic alogliptin benzoate crude product, heat and reflux for 20 minutes, press filter into the crystallization kettle of the fine drying bag and stir, and then press into the crystallization kettle Butyl ether, naturally cooled to room temperature, stirred and crystallized for 3.5 hours; the consumption of described methanol was equivalent to 5 times of the crude product quality of alogliptin benzoate; the consumption of described methyl tert-butyl ether was equivalent to benzoic acid 4.5 times the mass of alogliptin crude product;

[0050] (2) Centrifuge, wash the obtained solid with methanol, and blow dry at 50°C to obtain alogliptin benzoate polymorphic crystal product with a yield of 81.6% and a purity of 99.99%.

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Abstract

The invention relates to a preparation method for a benzoic acid alogliptin polycrystalline type crystal and belongs to the technical field of medicinal chemistry. The preparation method comprises the following steps: methyl alcohol is added into a reaction still and stirred, benzoic acid alogliptin crude product obtained after synthesis is added, heating reflux is carried out for 15-30 minutes, the benzoic acid alogliptin crude product is filter-pressed into a refining-drying-packing crystallization kettle and stirred, methyl tertiary butyl ether is pressed into the crystallization kettle, the mixture is subjected to natural cooling to the room temperature, stirring and crystallization for 3-4 hours and centrifugation to obtain a solid, and the solid is washed with methyl alcohol and dried at 45-55 DEG C through blasting to obtain the benzoic acid alogliptin polycrystalline type crystal. The obtained benzoic acid alogliptin polycrystalline type crystal is low in impurity content and higher in medicine quality.

Description

technical field [0001] The invention relates to a preparation method of alogliptin benzoate polymorph crystals, belonging to the technical field of medicinal chemistry. Background technique [0002] Diabetes mellitus is a series of clinical syndromes caused by absolute or relative insufficiency of insulin in the body. China is a big country with diabetes, and the absolute number of people with diabetes has always been the highest in the world. According to data from a paper published in the Journal of the American Medical Association that tracked the incidence of diabetes in China since 2010, the estimated prevalence of diabetes among adults aged 18 and over in my country was 11.6%, or about 113.9 million. Current medical research has confirmed that dipeptidyl peptidase Ⅳ (DPP-Ⅳ) inhibitor is a new type of diabetes treatment drug, by controlling glucagon-like peptide-1 (GLP-1) and glucose-dependent insulin-stimulating polypeptide ( The incretin activity of GIP, also known ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/04
CPCC07B2200/13C07D401/04
Inventor 杨汉跃郑家通董超陈学民王建涛
Owner JIANGSU DEYUAN PHARMA
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