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Aceclofenac synthesis refining process

A technology of aceclofenac and process, applied in the field of raw material drug synthesis, can solve the problems of many by-products, the purity of aceclofenac needs to be improved, etc., and achieve the effects of improving whiteness and improving purity

Pending Publication Date: 2021-01-22
陕西恒诚制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For the above-mentioned related technologies, the above-mentioned method produces more by-products, and the inventor believes that there is a defect that the purity of aceclofenac needs to be improved

Method used

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  • Aceclofenac synthesis refining process
  • Aceclofenac synthesis refining process
  • Aceclofenac synthesis refining process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A process for synthesizing and refining aceclofenac, comprising the following steps:

[0033] (1) Add 80ml of formic acid and 40g of tert-butyl aceclofenac to a three-necked flask, heat up to 72°C and keep warm, react for 4 hours, cool to normal temperature, filter with suction, wash with water, rinse in a centrifuge until the pH of the drain Above 5.0, centrifuge and dry to obtain 33g aceclofenac crude product;

[0034] (2) Put 33g of aceclofenac crude product into a beaker, add 19.8ml cyclohexane to cover the aceclofenac crude product, soak for 20min, stir and wash at a stirring speed of 30rpm, stirring time is 15min, centrifuge to dry, and dry at 80°C, Obtain 32.5g of aceclofenac, the refined yield is 98.5%, and the HPLC purity is 99.993%.

Embodiment 2

[0036] A process for synthesizing and refining aceclofenac, comprising the following steps:

[0037] (1) Add 80ml of formic acid and 40g of tert-butyl aceclofenac to a three-necked flask, heat up to 75°C and keep warm, react for 3 hours, cool to normal temperature, filter with suction, wash with water, rinse in a centrifuge until the pH of the drain Above 5.0, centrifuge to dry, obtain 32g aceclofenac crude product;

[0038] (2) Put 32g of aceclofenac crude product into a beaker, add 32ml of cyclohexane to cover the aceclofenac crude product, soak for 20min, stir and wash at a stirring speed of 30rpm, stirring time is 15min, spin dry by centrifugation, and dry at 80°C to obtain 31.7g of aceclofenac, the refined yield is 98.8%, and the HPLC purity is 99.985%.

Embodiment 3

[0040] A process for synthesizing and refining aceclofenac, comprising the following steps:

[0041] (1) Add 80ml of formic acid and 40g of tert-butyl aceclofenac to a three-necked flask, heat up to 78°C and keep warm, react for 3 hours, cool to normal temperature, filter with suction, wash with water, rinse in a centrifuge until the pH of the drain Above 5.0, centrifuge to dry, obtain 31g aceclofenac crude product;

[0042] (2) Put 31g of aceclofenac crude product into a beaker, add 46.5ml cyclohexane to cover the aceclofenac crude product, soak for 20min, stir and wash at a stirring speed of 30rpm for 15min, spin dry by centrifugation, and dry at 80°C. Obtain 30.4g of aceclofenac, the refined yield is 98.1%, and the HPLC purity is 99.986%.

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Abstract

The invention relates to the field of raw material medicine synthesis, and particularly discloses an aceclofenac synthesis refining process which comprises the following steps: (1) adding tert-butyl aceclofenac into formic acid, heating to perform acidolysis reaction, cooling to normal temperature, performing suction filtration, washing with water, leaching until the pH value of drained water is 5.0 or above, and performing centrifugal spin-drying to obtain an aceclofenac crude product; and (2) putting the aceclofenac crude product into a reaction container, adding an organic solvent to coverthe aceclofenac crude product, enabling the aceclofenac to be insoluble or slightly soluble in the organic solvent, soaking, stirring and washing, centrifugally spin-drying, and drying to obtain the aceclofenac. The process provided by the invention has the advantage of improving the purity and whiteness of aceclofenac.

Description

technical field [0001] The application relates to the field of raw material drug synthesis, more specifically, it relates to a process for synthesizing and refining aceclofenac. Background technique [0002] Aceclofenac, the chemical name is 2-((2,6-dichlorophenyl) amino) phenylacetoxyacetic acid, this product is a newly synthesized orally effective non-steroidal anti-inflammatory analgesic, belonging to benzene Acetic acid anti-inflammatory, antipyretic and analgesic drugs are structurally related to diclofenac, aclofenac and fenclofenac. In clinical practice, their pharmacological effects are compared with other non-steroidal drugs. , In the experimental model of chronic inflammation, it is characterized by obvious and extensive anti-inflammatory effects, strong analgesic and antipyretic effects, and gastric toxicity. [0003] A kind of preparation method of aceclofenac is disclosed in the related art, in the presence of triethylamine, diclofenac and tert-butyl bromoaceta...

Claims

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Application Information

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IPC IPC(8): C07C229/42C07C227/16C07C227/40
CPCC07C227/16C07C227/40C07C229/42
Inventor 白杨
Owner 陕西恒诚制药有限公司
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