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Selexipa crystal form and preparation method thereof

A technology of Selexipa and crystal form, which is applied in the field of medicine, can solve problems such as life-threatening and treatment, syncope, and right ventricular failure, and achieve the effects of reducing cost burden, low content of related substances, and prolonging the validity period

Active Publication Date: 2022-03-15
JIANGSU HANSOH PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are about 146,000 patients with pulmonary arterial hypertension in the world, and the incidence ratio of male to female is about 1:5, and it is more common in young women. Insufficient attention has eventually led to right ventricular failure and fatal syncope, endangering life and prognosis of treatment

Method used

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  • Selexipa crystal form and preparation method thereof
  • Selexipa crystal form and preparation method thereof
  • Selexipa crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0091] Example 1: Cyrexipa sample column chromatography treatment

[0092] Dissolve 20g of Selexipa sample in 200ml of dichloromethane, add 200g of silica gel (160-200 mesh), stir evenly, concentrate under reduced pressure to dry dichloromethane to obtain a sandy material, add 800g of silica gel ( 160-200 mesh), vibrate, add the above-mentioned sand material, 10L is eluted with ethyl acetate, and the eluate is concentrated to dryness under reduced pressure to obtain 15g of a light yellow sample.

Embodiment 2

[0093] Embodiment 2: the preparation of seed crystal

[0094]Add 1g of material treated by column chromatography into 18ml of isopropanol, heat to 83°C, all solids dissolve, cool to 70°C at a rate of 1°C / h, heat to 80°C, and then heat at 1°C / h The speed was cooled to 70° C., and so repeated for 12 cycles to obtain 0.91 g of Form A with a purity of 99.99%.

Embodiment 3

[0095] Embodiment 3: the preparation of crystal form A

[0096] Mix 2g of Selexipah sample treated by column chromatography with 18ml of isopropanol, heat to 83°C to dissolve all the samples, slowly cool down to 80°C, add 0.04g of seed crystals, keep stirring for 48 hours, and then Cool down to 70°C at a rate of °C / h, continue stirring for 24h, and filter to obtain 1.89g of Form A with a purity of 99.98%. Its X-ray diffraction pattern is as figure 1 shown. Its DSC spectrum is as figure 2 shown. Its TGA spectrum is as image 3 shown.

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Abstract

The present invention relates to a new crystal form of Selesipah with improved properties and a preparation method thereof. The method adopts a cyclic crystallization method to obtain a crystal form A of Selesipah. Compared with the traditional crystalline form of Selexipa, the crystalline form A of Selaxipa has a high melting point, good stability, high crystal purity, low content of related substances, mild process conditions, and is suitable for large-scale production, including this crystal form The pharmaceutical composition and dosage form can be used for treating pulmonary arterial hypertension.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a crystal form A of Selexipah and a preparation method thereof. Background technique [0002] Selexipa, the chemical name is 2-{4-[N-(5,6-diphenylpyrazin-2-yl)-N-isopropylamino]butyl}-N-(methylsulfonyl ) Acetamide, the English name is Selexipag, and the structural formula is as shown in formula (1): [0003] [0004] Selexipa is a new oral long-acting PGI2 receptor agonist jointly developed by Nippon Shinyaku and its licensed company Actelion, which is mainly suitable for the treatment of pulmonary arterial hypertension (PAH). Pulmonary hypertension is a clinical syndrome characterized by a progressive increase in pulmonary vascular resistance, which eventually leads to right heart failure and even death. There are about 146,000 patients with pulmonary arterial hypertension in the world, and the incidence ratio of male to female is about 1:5, and it is more comm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D241/20A61P9/12A61P11/00A61K31/4965
CPCC07D241/20A61P9/12A61P11/00C07B2200/13
Inventor 连小刚何雷林青周炳城
Owner JIANGSU HANSOH PHARMA CO LTD