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Method for preparing spherical baricitinib crystal

A crystallization and spherical technology, applied in the direction of organic chemistry, organic chemistry, etc., can solve the problem of high viscosity of baricotine and achieve good fluidity

Inactive Publication Date: 2019-02-26
WEIHAI GUANBIAO INFORMATION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Purpose of the invention: The present invention aims at the problem of high viscosity of the existing baricithi, and proposes a method for preparing spherical baricitic crystals

Method used

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  • Method for preparing spherical baricitinib crystal
  • Method for preparing spherical baricitinib crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1. Step 1 Add 10 g of Baricit into 100 ml of water, heat to 40°C to dissolve, prepare a solution with a concentration of 0.10 g / ml, cool to room temperature, and filter.

[0025] Step 2 Keep the temperature of the filtrate in the first step at 5°C, add 20ml of 95% ethanol under stirring, grow crystals at constant temperature for 1 hour, and stir at a stirring speed of 190 rpm.

[0026] The third step The solution obtained in the second step is cooled to -5°C and stirred while continuing to stir, and the constant temperature crystal growth is continued for 1.5 hours. Wherein, the cooling rate is 0.5° C. / minute, and the stirring speed is 190 revolutions / minute.

[0027] Step 4 Suction filtration, wash the filter cake with 95% ethanol solution, and dry the filter cake at 50°C. Debarix is ​​a spherical crystal, and its polarized light microscope photo is shown in the appendix figure 1 , D90 is 102μm, the purity detected by HPLC is 99.97%, and the yield is 93.24%. ...

Embodiment 2

[0029] Step 1 Add 25g of Baricit into 100ml of water, heat to 50°C to dissolve, prepare a solution with a concentration of 0.25g / ml, cool to room temperature, and filter;

[0030] Step 2 Keep the temperature of the filtrate in the first step at 15°C, add 30ml of 95% ethanol under stirring, grow the crystal at constant temperature for 2.5 hours, and stir at a stirring speed of 160 rpm;

[0031] The third step, the solution obtained in the second step, continued to stir, cooled to 0°C and stirred, and continued to grow crystals at a constant temperature for 2 hours, wherein the cooling rate was 1°C / min, and the stirring speed was 160 rpm;

[0032] Step 4 Suction filtration, wash the filter cake with 95% ethanol solution, and dry the filter cake at 60°C. Debarix is ​​a spherical crystal, and its polarized light microscope photo is shown in the appendix figure 1 , D90 is 74μm, the purity detected by HPLC is 99.99%, and the yield is 92.02%.

Embodiment 3

[0033] Example 3. In the first step, add 15g of Baricit into 100ml of water, heat to 45°C to dissolve, prepare a solution with a concentration of 0.15g / ml, cool to room temperature, and filter;

[0034] Step 2 Keep the temperature of the filtrate in the first step at 10°C, add 25ml of 95% ethanol under stirring, grow the crystal at constant temperature for 1.8 hours, and stir at a stirring speed of 178 rpm;

[0035] The third step The solution obtained in the second step, continue to stir, cool down to -2.5°C and stir, continue to grow crystals at a constant temperature for 1.8 hours, wherein, the cooling rate is 0.8°C / min, and the stirring speed is 178 rpm;

[0036] Step 4 Suction filtration, wash the filter cake with 95% ethanol solution, and dry the filter cake at 55°C. Debarix is ​​a spherical crystal, and its polarized light microscope photo is shown in the appendix figure 1 , D90 is 80μm, the purity detected by HPLC is 99.99%, and the yield is 92.98%.

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Abstract

The invention relates to a method for preparing a spherical baricitinib crystal. The method for preparing the spherical baricitinib crystal comprises the following steps: adding baricitinib into water, heating to 40-50 DEG C, dissolving, and filtering; keeping the filtrate at a temperature range of 5-15 DEG C, adding 95% ethanol which is 0.2-0.3 time of the volume of filtrate obtained at the firststep while stirring, culturing a crystal for 1-2.5 hours at a constant temperature, and stirring; continuously stirring, cooling to subzero 5 to 0 DEG C, continuously culturing the crystal for 1.5-2hours at the constant temperature, and stirring; carrying out suction filtration, washing filtrate cakes, and drying at 50-60 DEG C. By adopting the technical scheme of the invention, the spherical baricitinib crystal is obtained, and the spherical baricitinib crystal has very good flowability and is free of adhesion in the pressing process.

Description

technical field [0001] The invention relates to a preparation method of spherical baricotide crystals, which belongs to the technical field of raw material medicine preparation. Background technique [0002] Rheumatoid arthritis is a chronic, inflammatory synovitis-based systemic disease of unknown etiology. It is characterized by polyarticular, symmetrical, and aggressive arthritis of the small joints of the hands and feet, often accompanied by involvement of extra-articular organs and positive serum rheumatoid factor, which can lead to joint deformities and loss of function. According to statistics from relevant departments, the disability rate of rheumatoid arthritis in my country is as high as 70%. [0003] According to reports, the incidence of rheumatoid arthritis in our country is 0.3%-0.4%. If these rheumatoid arthritis patients are not treated effectively, the final impact will be lifelong disability, seriously affecting the patient's life and quality of life. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
CPCC07B2200/13C07D487/04
Inventor 不公告发明人
Owner WEIHAI GUANBIAO INFORMATION TECH
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