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Dezocine A crystal form and preparation method thereof

A technology of dezocine and crystal form, applied in the field of dezocine A crystal form and its preparation, can solve problems such as no crystal form involved, and achieve the effects of reducing product impurity content, good reproducibility and simple operation

Inactive Publication Date: 2017-12-29
JIANGSU HAICI BIOLOGICAL PHARMA CO LTD OF YANGTZE RIVER PHARMA GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Patent US3836670A and patent ZA8506680 describe the preparation process of dezocine and its preparations, but neither involves the crystal form

Method used

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  • Dezocine A crystal form and preparation method thereof
  • Dezocine A crystal form and preparation method thereof
  • Dezocine A crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In this embodiment, the method for preparing crystal form of dezocine A includes the following steps:

[0037] 1) Dissolve 10 g of crude dezocine in 100 ml of methanol, heat to reflux for 30 minutes, and filter while hot;

[0038] 2) Cool down to -5°C to charge the analytical crystals, filter and dry to obtain crude dezocine; obtain 6.5g off-white or white crystalline powder, with a yield of 65%.

[0039] Take the off-white crystalline powder obtained in Example 1 for structural analysis, and the results are as follows:

[0040] Its X-ray powder diffraction pattern is as follows figure 1 Shown.

[0041] The elemental analysis results were: C (%): 78.32, N (%): 5.70, H (%): 9.41, O (%): 6.52.

[0042] Its infrared spectrum (IR) diagram is as figure 2 Shown.

[0043] Its differential scanning thermal analysis chart (DSC chart) is as image 3 Shown.

[0044] The thermogravimetric (TG) diagram of Dezocine A crystal form is as follows Figure 4 Shown.

[0045] The HPLC detection method i...

Embodiment 2

[0049] In this embodiment, the method for preparing crystal form of dezocine A includes the following steps:

[0050] 1) Dissolve 10g of crude dezocine in 200ml of ethanol, heat to reflux for 30 minutes, and filter while hot;

[0051] 2) Cool down to 30°C to charge the analytical crystals, filter, and dry to obtain crude dezocine; obtain 7.5 g of off-white crystalline powder with a yield of 75%.

[0052] The structure analysis result of the product of Example 2 is not significantly different from the structure analysis result of Example 1.

[0053] The HPLC detection method is as in Example 1, HPLC diagram and Figure 5 Similar, no obvious difference, the enantiomer is not more than 0.2%.

[0054] The related substance detection method is as in Example 1. The related substance detection spectrum is Image 6 Show similar. Single impurity is not more than 0.05%, total impurity is not more than 0.3%.

Embodiment 3

[0056] In this embodiment, the method for preparing crystal form of dezocine A includes the following steps:

[0057] 1) Dissolve 10g of crude dezocine with 150ml of ethanol, heat to reflux for 30 minutes, and filter while hot;

[0058] 2) Cool down to 5-10°C to charge the analytical crystals, filter, and dry to obtain crude dezocine; obtain 8 g of off-white crystalline powder, with a yield of 80%.

[0059] The structure analysis result of the product of Example 3 is not significantly different from the structure analysis result of Example 1.

[0060] The HPLC detection method is as in Example 1, HPLC diagram and Figure 5 Similar, no obvious difference, the enantiomer is not more than 0.2%.

[0061] The related substance detection method is as in Example 1. The related substance detection spectrum is Image 6 Show similar. Single impurity is not more than 0.05%, total impurity is not more than 0.3%.

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Abstract

The invention provides a dezocine A crystal form. Cu-Kalpha ray radiation, X-ray powder diffraction represented by an angle 2theta has characteristic peaks at 9.261+ / -0.1, 11.142+ / -0.1, 12.334+ / -0.1, 13.007+ / -0.1, 14.068+ / -0.1, 14.709+ / -0.1, 15.142+ / -0.1, 18.538+ / -0.1, 19.420+ / -0.1, 19.675+ / -0.1, 23.218+ / -0.1, 24.720+ / -0.1, 25.710+ / -0.1, 27.183+ / -0.1, 28.081+ / -0.1, 28.348+ / -0.1 and 31.040+ / -0.1. The invention further provides a preparation method of the dezocine A crystal form. The dezocine A crystal form disclosed by the invention has extremely high bioavailability. The preparation method of the high-purity dezocine A crystal form disclosed by the invention has the technical effects that the impurity content is reduced, the individual impurity content is reduced from 0.15% to 0.05% or less, the total impurity content is reduced from 1.0% to 0.3% or less, the enantiomer content is not more than 0.2%, and the technical effect of simple and convenient operation is achieved.

Description

Technical field [0001] The invention relates to a crystal form of dezocine A and a preparation method thereof, and belongs to the technical field of medicine production. Background technique [0002] The chemical name of palrestat is: (-)-[5R-(5α,11α,13S*)]-13-amino-5,6,7,8,9,10,11,12-octahydro- The chemical structure of 5-methyl-5,11-methylenebenzocyclodecen-3-ol is as follows: [0003] [0004] Dezocine was developed by Sweden Astra. It is a potent opioid analgesic. It is a mixed agonist-antagonist of opioid receptors. It fully activates κ receptors and has a strong analgesic effect. It produces spinal analgesia, sedation and mild analgesia. The degree of respiratory depression only causes a weak effect on μ receptors, and sometimes due to the partial effect of anti-agonist drugs, it can be shown as a partial blocking effect, so there are fewer related side effects. Because of its strong analgesic effect and mild side effects, Dezocine is widely used for postoperative analgesia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/64C07C213/10A61K31/137A61P25/04
CPCC07C215/64C07B2200/13C07C213/10
Inventor 王庆辉牛明玉马立金张沛王伟胡丽娜朱圣红
Owner JIANGSU HAICI BIOLOGICAL PHARMA CO LTD OF YANGTZE RIVER PHARMA GRP
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