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Preparation method for synthesizing vanillin by using natural eugenol as raw material

A technology for vanillin and eugenol is applied in the field of preparation of natural eugenol as raw material for synthesizing vanillin, which can solve problems such as incomplete fragrance preparation technology, achieve reduced danger and toxicity, easy to scale up production and simple operation Effect

Inactive Publication Date: 2014-03-12
NANCHANG HANGKONG UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few domestic reports on the industrial production of vanillin using natural eugenol, and there is no complete synthesis of the preparation process for this spice

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of preparation method taking natural eugenol as raw material to synthesize vanillin, the process method steps are as follows:

[0022] 1. Preparation of Isoeugenol

[0023] In a 250mL three-neck round-bottomed flask equipped with a reflux condenser, a magnetic stirring device and a constant pressure dropping funnel, put 48.8g of potassium hydroxide and 70.6g of n-amyl alcohol into it, stir and dissolve to obtain a light yellow viscous liquid, add dropwise 20.0g of natural eugenol, heated at 80°C, and continued to react for 4 hours after the reflux temperature was 140°C, the solution gradually changed from light yellow to brown. Brown two layers, transfer the lower layer to a 250mL separatory funnel, then wash with 10% NaOH solution until the color of the upper layer no longer becomes lighter, combine the washed lye, extract with 80ml acetone, and remove organic matter containing n-pentanol. Phase, the extract was adjusted to pH = 4-5 with hydrochloric acid s...

Embodiment 2

[0029] A kind of preparation method taking natural eugenol as raw material to synthesize vanillin, the process method steps are as follows:

[0030] 1. Preparation of Isoeugenol

[0031] In a 250mL three-neck round-bottomed flask equipped with a reflux condenser, a magnetic stirring device and a constant pressure dropping funnel, put 48.8g of potassium hydroxide and 70.6g of n-amyl alcohol into it, stir and dissolve to obtain a light yellow viscous liquid, add dropwise 20.0g of natural eugenol, heated at 80°C, and continued to react for 4.5h after the reflux temperature was 145°C, the solution gradually turned from light yellow to brown. There are two light brown layers, transfer the lower layer to a 250mL separatory funnel, then wash with 13% NaOH solution until the color of the upper layer no longer becomes lighter, combine the washed lye, extract with 80ml acetone, and remove the n-pentanol-containing For the organic phase, the extract was adjusted to pH=4-5 with hydro...

Embodiment 3

[0037] A kind of preparation method taking natural eugenol as raw material to synthesize vanillin, the process method steps are as follows:

[0038] 1. Preparation of Isoeugenol

[0039] In a 250mL three-neck round-bottomed flask equipped with a reflux condenser, a magnetic stirring device and a constant pressure dropping funnel, put 48.8g of potassium hydroxide and 70.6g of n-amyl alcohol into it, stir and dissolve to obtain a light yellow viscous liquid, add dropwise 20.0g of natural eugenol, heated at 80°C, and continued to react for 5 hours after the reflux temperature was 150°C, the solution gradually changed from light yellow to brown. Brown two layers, transfer the lower layer to a 250mL separatory funnel, then wash with 15% NaOH solution until the color of the upper layer no longer becomes lighter, combine the washed lye, extract with 80ml acetone, and remove organic matter containing n-pentanol. Phase, the extract was adjusted to pH = 4-5 with hydrochloric acid s...

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Abstract

The invention discloses a preparation method for synthesizing vanillin by using natural eugenol as raw material. The preparation method comprises the following steps: adding potassium hydroxide and n-amyl alcohol into a three-neck round bottom flask with volume of 250 ml and equipped with a backflow condensation tube, a magnetic stirring device and a constant-pressure dropping funnel through isomerization, dropwise adding the natural eugenol after stirring for dissolution, heating for backflow, then transferring a reaction solution into water for dilution, transferring lower-layer liquid to a separatory funnel in several times, and washing with a NaOH solution until the color of upper-layer liquid does not become light; combining all alkali liquors, and extracting with acetone, acidating and evaporating rotatably to obtain isoeugenol; adding a certain amount of nitrobenzene into the isoeugeno to oxidize double bond of propenyl of the isoeugeno, and then purifying a vanillin crude product, wherein the vanillin productivity can reach above 95.0%. The method has the advantages that the adoption of highly-toxic catalysts of carbonyl iron and the like in the isomerization process is avoided, the after-treatment technology is relatively simple, and the operation is convenient. An extraction agent can be recycled to lower the cost.

Description

technical field [0001] The invention relates to a preparation method for synthesizing vanillin from natural eugenol, which belongs to the field of organic chemical synthesis. Background technique [0002] As a raw material and an important chemical intermediate, vanillin is also widely used in new flavors, food additives, and drug synthesis, so it has potential research and application values. At present, there are few domestic reports on the industrial production of vanillin using natural eugenol, and there is no complete synthesis of the preparation process for this spice. Contents of the invention [0003] The purpose of the present invention is to provide a kind of preparation method using natural eugenol as raw material to synthesize vanillin, taking natural eugenol as raw material, taking organic alcohol as reaction solvent, through alkali-catalyzed isomerization, dilution, alkali washing, extraction, Acidification yields isoeugenol. Then oxidize with an oxidant, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/58C07C45/27
CPCC07C41/32C07C45/27C07C47/58C07C43/23
Inventor 乐长高谢宇张二欢谢宗波李沐政
Owner NANCHANG HANGKONG UNIVERSITY
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