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Process for producing alpha-asarone raw material

A production process, the technology of asarone, applied in ether preparation, organic chemistry, etc., can solve the problems of low content of α-asarone, carcinogen safrole, and high extraction cost, so as to achieve excellent quality, increase yield, and reduce cost effect

Inactive Publication Date: 2004-07-14
刘博纯
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the low content of α-asarone isolated from the volatile oil of Shichangpu, the extraction cost is high, and it may also contain the carcinogenic substance safrole, and it cannot be mass-produced and applied clinically.

Method used

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  • Process for producing alpha-asarone raw material
  • Process for producing alpha-asarone raw material
  • Process for producing alpha-asarone raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Concrete production technique of the present invention comprises the following stages:

[0030] 1. Acetylation reaction stage

[0031] raw material name

Specification

Proportion amount(kg)

p-benzoquinone

Content ≥ 89%

1

Acetic anhydride

Content ≥ 94%

3

sulfuric acid

Content≥97%

0.2

water

8

[0032] (2), the technological process of acetylation reaction is as follows:

[0033] Brush and dry the 300L enamel reaction tank, check that the valve at the bottom of the tank is closed, vacuum pump in an accurate amount of 90kg of acetic anhydride, add 3.3L of sulfuric acid while stirring, adjust the temperature of the material in the tank to 40°C or 42°C, and start adding For p-benzoquinone in the ratio of raw materials, the feeding speed should be uniform and uninterrupted, and the temperature should be controlled at 45°C. After the addition, the temperature should be natu...

Embodiment 2

[0064] The technological process of methylation reaction can also use following method, and other stages are with embodiment one:

[0065] Pump quantitative water into a 500L enamel reaction kettle, add 1.2.4-triacetoxybenzene that meets the ratio of raw materials for methylation reaction, stir for 10 minutes, add liquid caustic soda that meets the ratio of raw materials for methylation reaction, and then drop Add dimethyl sulfate that meets the ratio of raw materials for the methylation reaction, adjust the pH value at 8 or 9 after dripping for 2 hours, carry out extraction, let stand to separate layers, separate the oil layer, extract the water layer again, combine the oil layers and add The extraction layer was washed with water until neutral, the water layer was discarded, the solvent was recovered, and distillation was continued, the fraction was collected at 145°C, and the vacuum was 0.1MPA to obtain a yellow or light yellow transparent liquid, namely 1.2.4-trimethoxybenz...

Embodiment 3

[0067] The technological process of methylation reaction can also use following method, and other stages are with embodiment one:

[0068] Pump a certain amount of water into a 500L enamel reaction kettle, add 1.2.4-triacetoxybenzene that meets the ratio of raw materials for the methylation reaction, stir for 10 minutes, add liquid caustic soda dropwise, add dimethyl sulfate dropwise, Then dropwise add liquid caustic soda, then dropwise add dimethyl sulfate, then dropwise add liquid caustic soda, liquid caustic soda and dimethyl sulfate that meet the raw material ratio of the methylation reaction are alternately added dropwise until the reaction is complete, and a stable reaction temperature is always maintained. Stable PH value state, mature reaction for 2 hours, extraction, standing to separate layers, separate the oil layer, extract the water layer again, combine the oil layer and the extraction layer, wash with water until neutral, discard the water layer, recover the solve...

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Abstract

The production process of alpha-asarone includes the following production stages: acetylation reaction, methylation reaction, hydroformylation reaction, vinylation reactin and re-crystallization. The artificial synthesis process of alpha-asarone has high yield of alpha-asarone, low cost, high purity up to 98.5 %, no carcinogenic substance safrole contained in the volatile oil, no toxic matter and no side effect and can meet clinical requirement.

Description

technical field [0001] The invention relates to a production process of an artificially synthesized crude drug, in particular to a production process of an alpha-asarone crude drug. Background technique [0002] α-Asarone is the active ingredient in the volatile oil of Calamus albus, after extraction, separation and pharmacological research, it is found that it has pharmacological effects such as relieving asthma, eliminating phlegm, relieving cough, calming, and reducing inflammation. Acute and chronic bronchitis caused by respiratory tract infection, Bronchitis, bronchial asthma, pneumonia, and intrapulmonary infection are common clinical diseases. They are frequently-occurring diseases with a long course of disease and recurrent attacks. There are many therapeutic drugs, but the therapeutic effect has not been satisfactory. It took a lot of energy and manpower to organize researchers to conduct in-depth discussions and research on this common disease, choose the best trea...

Claims

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Application Information

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IPC IPC(8): C07C41/01C07C43/243
Inventor 刘博纯
Owner 刘博纯
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