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Green synthesis process of berberine

A technology of green synthesis and synthesis process, which is applied in the field of green synthesis process of berberine, can solve the problems of hazards to operators and the environment, long synthesis route, and many preparation steps, so as to reduce process difficulty, reduce production cost, and improve reaction Yield effect

Inactive Publication Date: 2018-08-03
SICHUAN YIKE PHARMA CO LTD
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  • Application Information

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Problems solved by technology

[0006] In view of this, the application provides a green synthesis process of berberine, which solves the problems of producing a large amount of black polymers, many preparation steps, long synthesis routes, high toxicity of raw materials, and harm to operators and the environment in the existing synthesis process of berberine. problems such as hazards

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  • Green synthesis process of berberine

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Embodiment 1

[0027] Step 1): Synthesis of pepper rings

[0028] Take catechol 100g (0.2mol) and dissolve it in N,N-dimethylformamide (300g) and add it to the autoclave for nitrogen replacement, then add 500ml of aqueous solution in which 130g of potassium hydroxide is dissolved, fill it with nitrogen to 5atm, and stir Raise the temperature to 100-110°C and react for 3.5-4 hours. After the reaction, cool to room temperature, adjust the pH to 8, separate the liquids, extract the aqueous layer with 750ml*3 dichloromethane, combine the organic phases, dry, recover the solvent, and collect 172-174 ℃ / Hg distillate was light yellow pepper ring.

[0029] Step 2): the synthesis of piperonyl propionitrile

[0030] In a 2000ml four-necked bottle equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, add 270g of the pepper ring prepared in step 1), and add 300g of anhydrous aluminum trichloride in batches at ≤10°C under stirring, Control the temperature not to exceed 30°C,...

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Abstract

The invention discloses a green synthesis process of berberine. The synthesis process comprises the following steps: firstly, introducing dichloromethane into N,N-dimethylformamide by adopting catechol under the alkaline condition and reacting to synthesize benzodioxole; secondly, preparing pepper propionitrile by utilizing the obtained benzodioxole, preparing pepper propionamide by utilizing obtained pepper propionitrile, preparing homopiperony lamine by utilizing pepper propionamide and then synthesizing N-2,3-dimethoxybenzyl homopiperony lamine hydrochloride; finally, synthesizing berberinehydrochloride by utilizing the N-2,3-dimethoxybenzyl homopiperony lamine hydrochloride under the condition of glyoxal, formic acid and copper sulfate. The green synthesis process of the berberine, disclosed by the invention, has the advantages that the formation of black polymers is reduced, the reaction yield is improved, the problem that environmental pollution caused by a large amount of the black polymers produced in the original process production is solved and the requirements of green chemical synthesis required by China are met.

Description

technical field [0001] The invention relates to the technical field of green organic synthesis of pesticides, in particular to a green synthesis process of berberine. Background technique [0002] Berberine is an important alkaloid. It is a traditional Chinese medicine that has been used for a long time in my country. It can be extracted from plants such as Coptis chinensis, Cortex Phellodendri, Three Needles, and Shigonggong. It has a significant antibacterial effect. The commonly used berberine hydrochloride is also called Berberine hydrochloride and berberine can resist pathogenic microorganisms, and have inhibitory effects on Shigella, Mycobacterium tuberculosis, Pneumococcus, Typhoid bacillus and Diphtheria bacillus, among which the effect on Shigella is the strongest, and it is often used to treat bacillary dysentery , gastroenteritis and other digestive tract diseases, clinically mainly used for the treatment of bacillary dysentery and gastroenteritis, with few side eff...

Claims

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Application Information

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IPC IPC(8): C07D455/03
Inventor 安好义郑敏唐成贵安志远
Owner SICHUAN YIKE PHARMA CO LTD
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