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Veratryl alcohol preparation method

A technology of veratrol and veratrol, applied in the field of preparation of veratrol, can solve the problems of difficult separation, low product yield and high cost, and achieve the effects of improving conversion rate, shortening process flow and improving yield

Inactive Publication Date: 2017-12-12
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is exactly the problem of low product yield, difficult separation, and high cost in the preparation of veratrol in the prior art. It provides a kind of formaldehyde and veratraldehyde under the condition of basic catalyst to carry out cross Canny Zarrow reaction, improving the conversion rate of reactants and the production method of veratrol with simple process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Use 15wt% methylamine solution to adjust the pH value of the veratraldehyde solution to 8.5. In the veratraldehyde solution, in terms of mass percentage, the veratraldehyde is 48wt%, water is 49wt%, and the balance is impurities. The impurities mentioned therein are 3-methoxy-4-hydroxybenzaldehyde, dimethyl sulfate, catechol, veratrole, N,N-dimethylformamide and other substances;

[0024] (2) Slowly add the veratraldehyde solution treated in step (1) into a 1000ml three-necked flask containing formaldehyde solution with a constant pressure funnel, and 2 Under protection, the reaction is carried out at a temperature of 80° C. to prepare the crude product of veratrol.

[0025] (3) The crude product of veratrol obtained in step (2) is subjected to vacuum distillation under the conditions of an absolute pressure of 0.04 MPa and a temperature of 180° C. to obtain veratrol with relatively high purity.

[0026] After testing, the mass yield of veratrol was 88.35% based on...

Embodiment 2

[0028] (1) Use 15wt% propylamine solution to adjust the pH value of the veratraldehyde solution to 8.5. In the veratraldehyde solution, in terms of mass percentage, veratraldehyde is 78wt%, water is 20wt%, and the balance is impurities, wherein The impurities are 3-methoxy-4-hydroxybenzaldehyde, dimethyl sulfate, catechol, veratrole, N,N-dimethylformamide and other substances;

[0029] (2) Slowly add the veratraldehyde solution treated in step (1) into a 1000ml three-necked flask containing formaldehyde solution with a constant pressure funnel, and 2 Under protection, the reaction is carried out at a temperature of 80° C. to prepare the crude product of veratrol.

[0030] (3) The crude product of veratrol obtained in step (2) is subjected to vacuum distillation under the conditions of an absolute pressure of 0.04 MPa and a temperature of 180° C. to obtain veratrol with relatively high purity.

[0031] After testing, the mass yield of veratrol was 85.78% based on the amount of...

Embodiment 3

[0033] (1) Use 15wt% triethylamine solution to adjust the pH value of the veratraldehyde solution to 8.5. In the veratraldehyde solution, in terms of mass percentage, veratraldehyde is 49wt%, formaldehyde is 49wt%, and the balance is impurities , wherein the impurities mentioned are 3-methoxy-4-hydroxybenzaldehyde, dimethyl sulfate, catechol, veratrole, N,N-dimethylformamide and other substances;

[0034] (2) Slowly add the veratraldehyde solution treated in step (1) into a 1000ml three-necked flask containing formaldehyde solution with a constant pressure funnel, and 2 Under protection, the reaction is carried out at a temperature of 80° C. to prepare the crude product of veratrol.

[0035] (3) The crude product of veratrol obtained in step (2) is subjected to vacuum distillation under the conditions of an absolute pressure of 0.02 MPa and a temperature of 200° C. to obtain veratrol with relatively high purity.

[0036] After testing, during the 72h operation period, the mas...

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Abstract

The invention provides a veratryl alcohol preparation method and belongs to the technical field of alcohol preparation. The preparation process is as follows: (1) veratryl alcohol is further treated, and the solution pH is adjusted to 8-10; (2) the veratryl alcohol solution treated through the step (1) reacts with formaldehyde at a temperature of 60-85 DEG C, to obtain crude veratryl alcohol; and (3) the crude veratryl alcoholwas obtained in the step (2) is further purified. The crude veratryl alcohol prepared by using the method contains very few impurities, the impurities are separated easily, the veratryl alcohol is also a very important chemical raw material, the cost is reduced to a large extent, and the yield and purity of the veratryl alcohol are improved.

Description

technical field [0001] The invention relates to a preparation method of veratrol, in particular to a preparation method of veratrol, and belongs to the technical field of alcohol preparation. Background technique [0002] Veratrol (chemical name 3,4-dimethoxybenzyl alcohol, molecular formula C 9 h 12 o 3 ) referred to as VA, VA is a small molecular metabolite synthesized by white rot fungi in the secondary metabolism stage, and is an important raw material and intermediate for organic synthesis. It has the functions of sterilization, anti-cancer and anti-aging, and is generally used in the synthesis of drugs such as heart disease and high blood pressure. With the development of related industries, the demand for veratrol is increasing at home and abroad. [0003] The preparation method of the veratrol of existing veratrol mainly contains two kinds: a kind of is reduction method, such as sodium borohydride reduction method, with veratraldehyde as raw material, isopropanol...

Claims

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Application Information

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IPC IPC(8): C07C41/26C07C43/23
CPCC07C41/26C07C43/23
Inventor 于如军张振苗志伟郭玉娟王召滨陈艳艳
Owner SHANDONG UNIV OF TECH
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