Synthetic method of sodium houttuyfonate

A technology for the synthesis of houttuyfonate sodium and its synthesis method, which is applied in the field of synthesis of houttuyfonate sodium, which can solve the problems of expensive bromooctane, low total reaction yield, and no cost advantage, and achieve easy control of the reaction and simple operation steps , the effect of low production cost

Inactive Publication Date: 2017-01-11
SHANGHAI QINGPING PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the bromooctane used in this method is relatively expensive, and the total reaction yield of this method is low, so there is no cost advantage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0031] In a preferred embodiment, the synthetic method of above-mentioned houttuyfonate sodium comprises the following steps:

[0032] (1) Add the organic base and solvent into the reaction vessel, raise the temperature, and stir to dissolve; then, slowly add methylnonanone and ethyl formate to the reaction vessel, and control the temperature of the reaction system during the slow addition process. 50-70°C, and slowly add in 50-60 minutes; after that, cool the reaction system to 20°C±2°C, and keep the reaction at this temperature; then, further cool the reaction system to below 5°C, Insulate the reaction until the reaction is complete; then add cold water to the reaction vessel, stir and hydrolyze to obtain the intermediate I;

[0033] (2) Add the intermediate I and the solvent to another reaction vessel, cool to below 10°C, and then slowly feed SO 2 , Stir at 0~10℃, carry out addition reaction, post-treatment, and obtain houttuyfonate sodium product.

[0034] In a further p...

Embodiment 1

[0044] (1) Synthesis of intermediate I: Add 28kg sodium methoxide and 50kg toluene into a reaction kettle, heat up, stir and dissolve; The esters are slowly added to the reaction kettle. During the slow addition process, the temperature of the reaction system is controlled at 50-60°C, and the addition is completed slowly within 50-60 minutes; after the addition is completed, the reaction system is Cool to 20°C ± 2°C, and keep it warm at this temperature for 4 hours; then, further cool the reaction system below 5°C, keep it warm for 18 hours, and the reaction is complete; then add water temperature ≤ 5°C to the reaction kettle 350kg of cold water was stirred and hydrolyzed for 15 minutes, then left to stand for 30 minutes, separated, and the aqueous phase containing the prepared intermediate I was taken, transferred to another reaction kettle, and the toluene organic phase was recovered.

[0045](2) Synthesis of houttuyfonate sodium: Add the intermediate I and an appropriate am...

Embodiment 2

[0050] (1) Synthesis of intermediate I: Add 31kg sodium ethoxide and 50kg toluene into a reaction kettle, heat up, stir and dissolve; The esters are slowly added to the reaction kettle. During the slow addition process, the temperature of the reaction system is controlled at 60-70°C, and the addition is completed slowly within 50-60 minutes; after the addition, the reaction system Cool to 20°C±2°C, and keep it warm at this temperature for 5 hours; then, further cool the reaction system below 5°C, keep it warm for 20 hours, and the reaction is complete; then add water temperature ≤5°C to the reaction kettle 350kg of cold water was stirred and hydrolyzed for 15 minutes, then left to stand for 30 minutes, separated, and the aqueous phase containing the prepared intermediate I was taken, transferred to another reaction kettle, and the toluene organic phase was recovered.

[0051] (2) Synthesis of Houttuyfonate Sodium: Add the intermediate I and an appropriate amount of dichloromet...

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Abstract

The invention provides a synthetic method of sodium houttuyfonate. In the synthetic method, undecanone and ethyl formate are subjected to condensation reaction at low temperature and immediately hydrolyzed at low temperature to prepare an intermediate I, then SO2 and the intermediate I are subjected to an addition reaction, and finally the sodium houttuyfonate is prepared through simple aftertreatment. As sodium methylate and sodium ethoxide are adopted as alkali in the synthetic method, aftertreatment is convenient, operation steps are simple, and the requirement for equipment is low; sulfur dioxide is used as an addition agent, the reaction speed is high, reaction is easy to control, raw materials are easy to obtain, and the synthetic method is low in production cost and suitable for large-scale industrial production and has good application prospects and market potential.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a synthesis method of houttuyfonate sodium. Background technique [0002] The chemical name of sodium houttuyfonate is sodium decanoyl acetaldehyde bisulfite, and its structural formula is as follows: [0003] ; [0004] Sodium houttuyfonate (sodium houttuyfonate) is the sodium bisulfite adduct of decanoyl acetaldehyde, the active ingredient in natural Houttuynia cordata, which is artificially synthesized. Bacteria, Mycobacterium tuberculosis, etc. have a certain inhibitory effect, and can enhance the phagocytosis of leukocytes in the body and improve serum interleukin, so it can mobilize the body's immunity; it is usually used for anti-inflammatory and antibacterial, for example, for chronic bronchitis, chronic cervicitis, Annex inflammation, pneumonia in children, etc. Commercially available houttuyfonate sodium preparations include injections, tab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/32C07C309/08
CPCC07C303/32C07C45/72C07C309/08C07C49/24
Inventor 刘世领章强
Owner SHANGHAI QINGPING PHARMA CO LTD
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