Preparation technique of p-hydroxy-cinnamic acid

A technology for p-hydroxycinnamic acid and preparation technology, which is applied in the preparation of organic compounds, preparation of oxygenated compounds, chemical instruments and methods, etc., can solve the problems of difficult natural extraction methods, increased raw material costs, complex industrial production, etc. Ease of procurement, reduced energy consumption, and short response times

Inactive Publication Date: 2012-02-15
SHANDONG HOLLY PHARM CO LTD
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004]① The natural extraction method is difficult, costly and extremely low in yield;
[0005]② In the previous synthesis process, p-hydroxybenzaldehyde and malonic acid were used as raw materials, and p-hydroxycinnamic acid was synthesized according to the Knoevenagel-doebner reaction, but t

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0029] Example 1: Add 700ml ethyl acetate to a 2000ml four-necked flask, right

[0030] 97.6 g of hydroxybenzaldehyde was stirred and the temperature was lowered. When the temperature drops to 10-30°C, start adding 150g of sodium methoxide and control the temperature to 20-50°C. After the addition, stir and keep it at 20-50℃ for 8 hours. After the reaction is finished, add 200-500ml of water and stir for 15 minutes to start distillation. Distillate starts at around 65℃ until it reaches 99℃. After the distillation is finished, the temperature is lowered to below 50°C, and 600ml of 20% liquid caustic soda is slowly added, and then heated to reflux and kept for 2 hours. After the incubation, the temperature is lowered to 60°C, and 30% hydrochloric acid is slowly added dropwise. Adjust PH=1, lower the temperature to below 40°C, filter, wash the filter cake with water, and drain. After drying, 110-125g of finished product can be collected, with a content of more than 99%, and its a...

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PUM

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Abstract

The invention discloses a preparation technique of p-hydroxy-cinnamic acid, which comprises the following steps: carrying out reaction on p-hydroxy-benzaldehyde, which serves as the main raw material, under the catalytic action of sodium methoxide by using ethyl acetate as a solvent, thereby implementing experimentation and production by a one-step process; and after the reaction finishes, recycling the ethyl acetate, and carrying out alkali dissolution and acid precipitation to obtain the finished product, wherein the product purity is higher than 99%, and the mol yield is higher than 90%.

Description

technical field [0001] The invention specifically relates to a preparation process of p-hydroxycinnamic acid. Background technique [0002] P-Hydroxycinnamic acid (P-Hydroxycinnamic acid), also known as p-coumaric acid. Widely present in plants in nature, especially in leguminous plants. p-Hydroxycinnamic acid is widely used in chemical fields such as medicine, food, daily necessities, and feed. In terms of medicine, a large number of studies have shown that p-hydroxycinnamic acid has strong biological activities, such as anti-oxidation, anti-tumor, anti-chemotherapy and whitening effects, and it is also an active ingredient that benefits eyes. Oxyacids are similar, and have the advantages of moderate and long-lasting effects. They can also be used as intermediates in the production of coronary heart disease treatment drug Kexinding, as well as in the manufacture of local anesthetics, bactericides and hemostatic drugs. P-hydroxycinnamic acid is a very important flavor an...

Claims

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Application Information

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IPC IPC(8): C07C59/52C07C27/02
Inventor 李兰花裘月南吴华强王建荣
Owner SHANDONG HOLLY PHARM CO LTD
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