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Preparation technology of veratric acid

A preparation process, the technology of veratronic acid, which is applied in the preparation of carboxylate, the preparation of organic compounds, organic chemistry, etc., can solve the problems of expensive raw materials and low yield, and achieve the effect of reducing raw material costs and improving production efficiency

Active Publication Date: 2014-07-23
SHANDONG HOLLY PHARM CO LTD
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  • Summary
  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

The main disadvantage of this method is that
[0005] The raw materials are relatively expensive, and the reaction often produces an indeterminate by-product veratraldehyde, and the yield is generally not very high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Add 300-800ml of water into a 1000ml four-neck flask at room temperature,

[0021] 60g of veratraldehyde was heated to 40°C and stirred for 10 minutes until the veratraldehyde was completely melted. Then add 50-90ml of 30% liquid caustic soda and stir for 15 minutes. Slowly add 180ml of hydrogen peroxide at 40°C, and control the temperature at 30-35°C. The temperature will rise during the dropwise addition, and the addition will be completed in 3-5 hours. After adding the hydrogen peroxide, stir for 30 minutes, then raise the temperature to 55°C, and keep the temperature for 2 hours. Then raise the temperature to 60°C and keep it warm for 3 hours, then take samples for measurement; the result to be measured contains more than 99.2% of veratraldehyde, and when the content of veratraldehyde is less than 0.5%, cool down to below 25°C, use 300ml of water and 30% hydrochloric acid to slowly Adjust PH=2, about 2-4h or so. Filter, wash the filter cake with clean...

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PUM

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Abstract

The invention discloses a preparation process of veratronic acid, which mainly uses veratraldehyde as the main raw material, uses water as the solvent, forms a salt with alkali, oxidizes with hydrogen peroxide, and acidifies to obtain veratronic acid, and uses an organic solvent as the The solvent method greatly reduces the cost of raw materials and greatly improves the production efficiency, and the detection target content reaches more than 95%, and the liquid phase content reaches more than 99.5%.

Description

technical field [0001] The invention specifically relates to a preparation process of veratronic acid. Background technique [0002] Veratrol can be extracted from the seeds of Trollius chi-nenisi Baill., Zygadenus, Veratrum and Schoeno-caulon offricinale plants, and is mainly used as a chemical reagent . Veratronic acid is a commonly used intermediate in chemical synthesis, widely used in industry, medicine, pesticide and other fields, and is a key intermediate in the synthesis of drugs such as alfuzosin hydrochloride. [0003] The shortcoming that the preparation technology of veratrol in the past exists: [0004] ① Mainly use veratrol as raw material to produce veratrol through oxidation. The main disadvantage of this method is that [0005] The raw materials are relatively expensive, and the reaction often produces an indeterminate by-product veratraldehyde, and the yield is generally not very high. [0006] ②Using veratraldehyde as the starting material and methan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C65/21C07C51/285
Inventor 李兰花裘月南吴华强沈林华王建荣
Owner SHANDONG HOLLY PHARM CO LTD
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