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Purification method of pranoprofen

A technology of refining and purifying methanol water solution, which is applied in the field of preparation of non-steroidal anti-inflammatory drugs, can solve the problems of long cycle, increased production cost, and ineffective separation of pranoprofen impurity C.

Active Publication Date: 2019-10-25
GUANGZHOU HANPU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One is to strictly control the purity of starting materials, intermediates, reagents, etc., and strictly control reasonable reaction conditions and process parameters. The products obtained in this way are generally high in purity and low in impurity content, but the preparation process needs to be fully verified. , and the production process has many steps, a long cycle, and the operation is very difficult; the second is to repeat the recrystallization operation, usually recrystallization can play the effect of impurity removal and purification, but this operation is not obvious to the separation effect of pranoprofen impurity C, The repeated recrystallization operation greatly reduces product yield and production efficiency, and repeated recrystallization can cause 10%-20% loss; the third is to utilize the characteristics of pranoprofen containing carboxyl structure, and purify it with the method of alkali dissolution and acid analysis Refining can also effectively reduce the content of various impurities, but the material loss in the alkali-dissolving and acid-forming process is greater, and the loss in one operation cycle can reach 20%-30%, the product yield is greatly reduced, the production efficiency is low, and the production cost is increased.
[0006] In the current technology, there is still no simple, low-cost pranoprofen refining and purification method, so that the prepared pranoprofen can reach the expected quality requirements and continue to meet the safety, effectiveness and quality control of the drug sexual requirements

Method used

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  • Purification method of pranoprofen
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  • Purification method of pranoprofen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]Grind the pranoprofen to be treated and pass through a 60-mesh sieve, add 10 times the amount of 30% methanol aqueous solution, heat up to 50 ° C, keep stirring for 3 hours, cool to room temperature (25 ° C), filter, and use a small amount of the same The filter cake is rinsed with concentrated methanol aqueous solution, drained, and dried at low temperature, and the beating yield is 96.5%. Take the pranoprofen that has been beaten, add 35 times the amount of 50% methanol aqueous solution and put it in the decolorization tank, heat and stir to dissolve it, reflux for 10 minutes, filter it to the crystallization tank while it is hot, cool to 20 ° C, and crystallize for 5 Hour. Filter, rinse the crystals with a small amount of recrystallization solvent (50% methanol solution), drain, and dry at 50°C to obtain the finished product of pranoprofen. The impurity chromatogram of the product is as follows figure 2 As shown, its chromatographic purity is 99.75%, wherein the im...

Embodiment 2

[0045] Grind the pranoprofen to be treated and pass through an 80 mesh sieve, add 8 times the amount of 50% aqueous methanol solution, heat up to 60°C for reflux and keep stirring for 4 hours, cool to room temperature, filter, and use a small amount of methanol of the same concentration- The filter cake was rinsed with aqueous solution, drained, and dried at low temperature. The beating yield was 94.7%. Take the pranoprofen that has been beaten, add 25 times the amount of 50% methanol aqueous solution and put it in the decolorization tank, heat and stir to dissolve it, reflux for 30 minutes, filter it to the crystallization tank while it is hot, cool to 25 ° C, and crystallize for 5 Hour. Filter, rinse the crystals with a small amount of recrystallization solvent (50% methanol solution), drain, and dry at 55°C to obtain the finished product of pranoprofen. The impurity chromatogram of the product is as follows image 3 As shown, its chromatographic purity is 99.80%, wherein ...

Embodiment 3

[0049] Grind the pranoprofen to be treated and pass through a 100 mesh sieve, add 6 times the amount of 70% methanol solution, heat up to 50-60°C, keep stirring for 3 hours, cool to room temperature, filter, and rinse with a small amount of 70% methanol solution The filter cake is drained and dried at low temperature, and the beating yield is 88.7%. Take the pranoprofen that has been beaten, add 30 times the amount of 50% methanol aqueous solution, put it in the decolorization tank, heat it while stirring to dissolve, reflux for 10-30 minutes, filter it into the crystallization tank while it is hot, and cool it to 20-25 °C , crystallization for 5 hours. Filter, rinse the crystals with a small amount of recrystallization solvent, drain them, and dry them below 55°C to obtain the finished product of pranoprofen. The impurity chromatogram of the product is as follows Figure 4 As shown, its chromatographic purity is 99.75%, wherein the content of impurity A is 0.11%, the conten...

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Abstract

The invention discloses a purification method of pranoprofen, and relates to the field of preparation of nonsteroidal anti-inflammatory drugs. The problem that a simple, practicable and low-cost purification method of the pranoprofen does not exist in the prior art, and consequently the prepared pranoprofen cannot reach the expected quality requirements is solved. According to the technical key point, the purification method comprises the following steps that (1) beating is conducted, specifically, pranoprofen powder is added in a methanol aqueous solution, the temperature is risen to 50-60 DEG C, stirring is conducted for 3-5 hours under the temperature, and serous liquid is obtained; (2) the serous liquid is filtered; and (3) the pranoprofen obtained through filtering is mixed with the methanol aqueous solution and is dissolved, filtering, devitrification and drying are conducted while the solution is hot, and the f pranoprofen finished product is obtained. According to the purification method of the pranoprofen, operation is easy and convenient, and the prepared pranoprofen is high in purity, low in impurity content and high in yield.

Description

technical field [0001] The invention relates to the field of preparation of non-steroidal anti-inflammatory drugs, in particular to a method for refining and purifying pranoprofen. Background technique [0002] Pranoprofen belongs to propionic acid non-steroidal anti-inflammatory drugs, its mechanism of action is to mainly inhibit the activity of cyclooxygenase (COX), block the synthesis of eicosadonic acid derivatives, inhibit the synthesis of prostaglandins, relieve Inflammation. Its anti-inflammatory effect is stronger than aspirin and ibuprofen, etc., and the adverse reaction rate is low and mild. Clinically, it is mainly used locally for symptomatic treatment of the outer eye and front of the eye, such as blepharitis, conjunctivitis, keratitis, scleritis, superficial scleritis, iridocyclitis; oral administration is suitable for (1) chronic rheumatoid arthritis , Anti-inflammatory and analgesic for osteoarthritis, low back pain, periarthritis of shoulder, neck, shoulde...

Claims

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Application Information

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IPC IPC(8): C07D491/052
CPCC07D491/052
Inventor 饶汉才黄能章王硕刘志陈亮辉
Owner GUANGZHOU HANPU PHARM CO LTD
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