Refining method of cyclobenzaprine hydrochloride

Abstract

The invention discloses a refining method of cyclobenzaprine hydrochloride, and concretely relates to the field of medicines. The refining method comprises the following preparation steps: S1, in an extraction process in the later period of cyclobenzaprine hydrochloride processing, adding dispersed adsorption powder into a mixed solution of cyclobenzaprine hydrochloride, stirring by adopting a paddle stirrer, and precipitating to obtain a cyclobenzaprine hydrochloride crude product; S2, adding an organic solvent into the cyclobenzaprine hydrochloride crude product, performing recrystallization, dissolving and stirring in a steam pressurizing manner, and keeping constant temperature for later use; and S3, filtering and adsorbing the mixed solution obtained in step S2 through vesuvianite, and filtering to obtain a white refined cyclobenzaprine hydrochloride product. By adding the dispersed adsorption powder, crystals can be dispersed and fluffy, impurity byproducts are not wrapped, crystal discharging is fine and uniform, impurities and redundant metal ions can be adsorbed, and the cyclobenzaprine hydrochloride fine product with high purity and extraction rate is obtained.

Description

technical field [0001] The embodiments of the present invention relate to the field of medicine, in particular to a method for refining cyclobenzaprine hydrochloride. Background technique [0002] Cyclobenzaprine hydrochloride (cyclobenzaprine hydrochloride), the chemical name is 5-(3-dimethylaminopropylene)-dibenzo[a,e]cycloheptatriene hydrochloride, which is a muscle relaxant developed by Merck Company of the United States. Chi agent. The drug is clinically used to relieve muscle spasms and the accompanying severe pain of skeletal muscles without interfering with the normal function of muscles, and has been listed in TOP200 for many years. [0003] The Chinese invention patent with the patent public number of CN 101260046A discloses a refining method of cyclobenzaprine hydrochloride, which is to recrystallize with isopropanol first, and then wash with acetone, ether or tetrahydrofuran until off-white, although this method can obtain off-white White crystals, the polysodi...

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Problems solved by technology

[0003] The Chinese invention patent with the patent public number of CN 101260046A discloses a refining method of cyclobenzaprine hydrochloride, which is to recrystallize with isopropanol first, and then wash with acetone, ether or tetrahydrofuran until off-white, although this method can obtain off-white White crystals, the polysodium chloride impurities produced in the crystals can be separated and removed by being insoluble in ether / ethyl acetate mixture, but because they are first recrystallized and then filtered to remove impurities, the impurities will be wrapped when the crystals are precipitated In the middle of the crystal, difficult to remove;

[0004] The Chinese invention patent whose public number is CN 102976955A discloses a method for refining cyclobenzaprine hydrochloride. The patent uses acetone as the recrystallization solvent, and its boiling point and viscosity are much lower than that of isopropanol. Water and acetone are filtered while hot during recrystallization, and impurities are removed by adding activated carbon and silica gel, but there are still impurities in the obtained cyclobenzaprine hydrochloride crystals, and the boiling point of anhydrous acetone is low, which may volatilize when heated slightly Affect the purification rate

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