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A kind of azaspirone pharmaceutical composition and preparation method thereof

A composition and compound technology, applied in the directions of drug combination, drug delivery, pharmaceutical formulation, etc., to achieve the effect of reducing adverse reactions, shortening production cycle, and low content of related substances

Active Publication Date: 2021-09-17
SICHUAN CREDIT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are currently no relevant literature reports on the causes of the above adverse reactions

Method used

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  • A kind of azaspirone pharmaceutical composition and preparation method thereof
  • A kind of azaspirone pharmaceutical composition and preparation method thereof
  • A kind of azaspirone pharmaceutical composition and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 1. Preparation of cis-exo-bicyclo[2.2.1]heptane-2,3-dicarboximide

[0047] The cis-exo-bicyclo[2.2.1]heptane-2,3-dicarboximide was prepared according to the method reported in the literature (China New Technology and New Products. 2014, 8, 13), which was measured by HPLC. The content of related substances is 2.7%. Among them, HPLC (high performance liquid chromatography) test conditions are: use octadecylsilane bonded silica gel as filler, 0.01mol / L potassium dihydrogen phosphate solution (adjust pH to 7.5 with 10% sodium hydroxide solution)-acetonitrile (80:20) is the mobile phase, the detection wavelength is 243 nm, and the purity of the measured result is 97.3%.

[0048] 2. Purification of cis-exo-bicyclo[2.2.1]heptane-2,3-dicarboximide

[0049] (i) Weigh 100.0 g of cis-exo-bicyclo[2.2.1]heptane-2,3-dicarboximide prepared in the above step 1, add a mixed solvent of 400 mL of ethanol and 400 mL of water, and heat until the solvent is refluxed , after stirring for 1...

Embodiment 2

[0058] Using the cis-exo-bicyclo[2.2.1]heptane-2,3-dicarboximide prepared under the conditions 1-5 in Table 1 as raw materials, tandospirone citrate was prepared according to the above method The composition was detected by HPLC, and the content of tandospirone citrate was all above 98.0%, and the content of related substances was shown in Table 2.

[0059] Table 2. Test results

[0060]

[0061]

[0062] Note: "--" means not detected.

[0063] From the above content, it can be seen that the purification process of the intermediate cis-exo-bicyclo[2.2.1]heptane-2,3-dicarboximide in Examples 1 and 2 uses environmental protection, safety, low toxicity / non-toxicity and has the advantages of high yield and high purity; in addition, the preparation of the tandospirenone composition adopts a two-step one-pot process, which does not need to separate the intermediate products generated by the reaction, which greatly improves the industrial production efficiency and shortens the...

Embodiment 3

[0065] 1. The preparation of cis-exo-bicyclo[2.2.1]heptane-2,3-dicarboximide is the same as in step 1 of Example 1.

[0066] 2. Purification of cis-exo-bicyclo[2.2.1]heptane-2,3-dicarboximide

[0067] (i) Weigh 100.0 g of cis-exo-bicyclo[2.2.1]heptane-2,3-dicarboximide prepared in the above step 1, add a mixed solvent of 400 mL of ethanol and 400 mL of water, and heat until the solvent is refluxed , stirred for 1 h, cooled to room temperature naturally, placed at -10 ± 5 °C for 2 to 3 h, suction filtered, added a mixed solvent of 200 mL of ethanol and 200 mL of water to the filter cake, heated to solvent reflux, stirred for 1 h, naturally cooled to room temperature, Place at 5±5°C for 2-3 hours, filter, and dry the filter cake to obtain 99.5 g of cis-exo-bicyclo[2.2.1]heptane-2,3-dicarboximide with a yield of 99.5%. The purity measured by HPLC was greater than 99.5%, and the detection conditions were the same as in step 1 of Example 1, wherein the impurity 1 (cis-exo-bicyclo[...

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Abstract

A pharmaceutical composition of azaspireones and a preparation method thereof, the pharmaceutical composition of azaspirones comprises compound I and / or its citrate, compound II and / or its citrate and compound III And / or its citrate, which has anti-anxiety and anti-depressant effects and less adverse reactions; the product prepared by the preparation method has high purity and low content of related substances.

Description

technical field [0001] The present invention relates to an azaspipirone pharmaceutical composition and a preparation method thereof. Background technique [0002] Tandospirone belongs to the class of azaspirones with the chemical name (3aα,4β,7β,7aα)-hexahydro-2-[4[4-(2-pyrimidinyl)-1-(piperazinyl)- Butyl]-4,7-methylene-1H-isoindole-1,3(2H)-dione. It is a serotonin receptor agonist and belongs to the third generation of anxiolytics, mainly used to treat anxiety or other disorders associated with anxiety states. Tandospirone can be highly selectively and concentrated in the brain limbic system such as the hippocampus, septum, interpeduncular nucleus, amygdala and 5-HT in the suture gland nucleus of the emotional center. 1A Receptor binding, activating 5-HT 1A Autoreceptors, exert anxiolytic effects. Tandospirone can also exert some antidepressant effects at the same time. [0003] Compared with its similar derivative buspirone, tandospirone has a higher selective anxioly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K31/506A61P25/22A61P25/24C07D209/76
CPCA61K31/506C07D209/94A61K9/2059A61K9/2054A61K9/1652A61K9/0002A61K9/006C07B2200/07A61K2300/00
Inventor 陈刚李晓莉刘志鸿傅霖
Owner SICHUAN CREDIT PHARMA