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Production method for daidzein

A production method, the technology of daidzein, applied in the field of medicine, can solve the problems of expensive raw materials, strong irritation and strong corrosion of raw materials, and achieve the effect of easy-to-obtain raw materials, easy operation and mild reaction conditions

Inactive Publication Date: 2016-08-17
WUHU BAOPING INTELLIGENT SERVICE OUTSOURCING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] There are many ways to synthesize daidzein, and generally there are several methods as follows: using the zinc chloride / phosphorus oxychloride method, the yield of this method is only about 20%, and the raw materials are highly irritating and corrosive; using boron trifluoride Diethyl ether solution replaces anhydrous zinc chloride, and methyl chlorosulfonic acid is catalyzed to cyclize with dimethylformamide. The yield of this method is about 40%. The purity of raw materials is strict and the experimental process is difficult to control; triethyl orthoformate is used Cyclization synthesis method, the method conditions are mild, but the yield is only 25%; it is synthesized by triazine cyclizer, the raw material is expensive and the supply is in short supply, it is a general synthesis method of isoflavones, and it is not suitable for daidzein
After comparison, using resorcinol and p-hydroxyphenylacetic acid as raw materials, through anhydrous zinc chloride catalyzed condensation, dimethylformamide dimethyl acetal one-carbon unit transfer agent cyclization to generate daidzein, the product yield The yield is as high as 43.0%, and the quality basically meets the pharmacopoeia standard, but the yield of the product still needs to be further improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A production method of daidzein, comprising the following steps:

[0035] a. Condensation reaction:

[0036] Step 1: Check the reaction kettle. It should be dry and anhydrous. Mix 75kg of p-hydroxyphenylacetic acid, 75kg of resorcinol and 50kg of zinc chloride and add it to the reaction kettle. The reaction kettle is a 200L enamel kettle. Heat with steam, and start stirring when the material at the bottom of the kettle starts to melt. After the material in the kettle is completely dissolved, start the vacuum valve, control the vacuum degree above 0.08MPa, and control the temperature at 140°C. React for 20 minutes, and close the vacuum valve after the reaction is completed;

[0037] Step 2: Add 150L of dissolving water to the reactant, cool the interlayer of the reactor with cold water until the temperature in the reactor reaches below 30°C, stir and crystallize for 2 hours, put it in a centrifuge to dry, and collect the mother liquor, use 150L for the filter cake After...

Embodiment 2

[0053] A production method of daidzein, comprising the following steps:

[0054] a. Condensation reaction:

[0055] Step 1: Check the reaction kettle. It should be dry and anhydrous. Mix 75kg of p-hydroxyphenylacetic acid, 75kg of resorcinol and 50kg of zinc chloride and add it to the reaction kettle. The reaction kettle is a 200L enamel kettle. Heat with steam, and start stirring when the material at the bottom of the kettle starts to melt. After the material in the kettle is completely dissolved, start the vacuum valve, control the vacuum degree above 0.08MPa, and control the temperature at 136°C. React for 20 minutes, and close the vacuum valve after the reaction is completed;

[0056] Step 2: Add 150L of dissolving water to the reactant, cool the interlayer of the reactor with cold water until the temperature in the reactor reaches below 30°C, stir and crystallize for 2 hours, put it in a centrifuge to dry, and collect the mother liquor, use 150L for the filter cake After...

Embodiment 3

[0072] A production method of daidzein, comprising the following steps:

[0073] a. Condensation reaction:

[0074] Step 1: Check the reaction kettle. It should be dry and anhydrous. Mix 75kg of p-hydroxyphenylacetic acid, 75kg of resorcinol and 50kg of zinc chloride and add it to the reaction kettle. The reaction kettle is a 200L enamel kettle. Heat with steam, and start stirring when the material at the bottom of the kettle starts to melt. After the material in the kettle is completely dissolved, start the vacuum valve, control the vacuum degree above 0.08MPa, and control the temperature at 145°C. React for 20 minutes, and close the vacuum valve after the reaction is completed;

[0075] Step 2: Add 150L of dissolving water to the reactant, cool the interlayer of the reactor with cold water until the temperature in the reactor reaches below 30°C, stir and crystallize for 2 hours, put it in a centrifuge to dry, and collect the mother liquor, use 150L for the filter cake After...

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PUM

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Abstract

The invention provides a production method for daidzein. Hydroxyphenylacetic acid serves as a raw material, a crude product is obtained after a condensation reaction and a cyclization reaction, and then the final product is obtained after refining. The production method for daidzein is suitable for industrial production, the raw material is easy to obtain, reaction conditions are mild, operation is easy, the yield of the product can reach 55% or above, and the purity of the product is larger than or equal to 99%.

Description

technical field [0001] A production method of daidzein belongs to the field of medicine. Background technique [0002] There are many ways to synthesize daidzein, and generally there are several methods as follows: using the zinc chloride / phosphorus oxychloride method, the yield of this method is only about 20%, and the raw materials are highly irritating and corrosive; using boron trifluoride Diethyl ether solution replaces anhydrous zinc chloride, and methyl chlorosulfonic acid is catalyzed to cyclize with dimethylformamide. The yield of this method is about 40%. The purity of raw materials is strict and the experimental process is difficult to control; triethyl orthoformate is used The cyclization synthesis method has mild conditions, but the yield is only 25%. It is synthesized using a triazine ring-synthesizing agent, and the raw materials are expensive and in short supply. It is a general synthesis method for isoflavones and is not suitable for daidzein. After compari...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/36
CPCC07D311/36
Inventor 沈少银袁玲肖兴亮王军沈刚圣荔
Owner WUHU BAOPING INTELLIGENT SERVICE OUTSOURCING CO LTD