Heliotropin decolorizer and preparation method of heliotropin

A technology of jasmonal and aldehyde decolorizing agent, which is applied in the direction of organic chemistry to achieve the effect of good appearance and strong fragrance of the product

Inactive Publication Date: 2011-08-17
重庆德馨香料植物开发有限公司
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the jasminal that above-mentioned method obtains is yellow, and wherein contains nitro compound impurity

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0026] The preparation of jasmonal crude product can adopt method as follows:

[0027] A. Condensation reaction 3,4-dioxymethylene mandelic acid

[0028] Under the condition of -20-0℃, pH 1-3, piperonyl ring reacts with glyoxylic acid to generate 3,4-dioxymethylene mandelic acid;

[0029] B. Oxidative synthesis of crude jasmonal

[0030] Carry out oxidative decarboxylation of 3,4-dioxymethylene mandelic acid with nitrate in boiling water to obtain the crude product of jasmonal, the nitrate oxidizing agent is silver nitrate, the nitrite is sodium nitrite, both It can be used in combination as an oxidizing agent.

[0031] But the present invention is not limited to the above method for preparing the crude jasmonal, and other methods can also be used, as long as the prepared jasmonal crude contains nitro compound impurities.

Embodiment 1

[0032] The preparation method of embodiment 1 jasron decolorizing agent and jasmonal

[0033] Add the water that is equivalent to 0.5 times of the weight of the jasronal crude product in the jasronal crude product gained through nitrite oxidation, obtain the jasronal aqueous solution, add the jasronal decolorizing agent that mass concentration is 1% in the jasronal aqueous solution, The jasmonal decolorizing agent contains 10 parts by weight of thiourea dioxide and 3 parts of sodium hydroxide, stirred evenly, heated to 80-95°C and kept warm until the reaction is complete, allowed to stand for stratification, and removed the supernatant and the bottom layer. Contains jasmonal decolorizing agent, the residue is collected at -0.1MPa, 140-145°C, and the collected product is jasmonal, which is a white crystal. The white crystal is jasmonal, and the yield is 85.8 %;

[0034] The yield of jasmine aldehyde of white crystals prepared by other methods is usually 65%.

Embodiment 2

[0036] In the jasronal crude product oxidized by nitrite, add water equivalent to 3 times of the jasronal crude product weight to obtain a jasronal aqueous solution, and add a jasronal decolorizing agent with a mass concentration of 15% in the jasronal aqueous solution, so that The said jasmonal decolorizer contains 10 parts by weight of thiourea dioxide and 13 parts of sodium hydroxide, stirs evenly, heats to 80-95 ° C and keeps warm until the reaction is complete, puts it to stratification, removes the supernatant and the bottom layer containing The jasronal decolorizing agent, the residue was collected at -0.1MPa, 140-145°C, and the collection was jasronal, which was a white crystal. The white crystal was jasmonal, and the yield was 86%. ;

[0037] The yield of jasmine aldehyde of white crystals prepared by other methods is usually 65%.

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PUM

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Abstract

The invention relates to the field of chemical synthesis. Concretely, a heliotropin decolorizer consists of water-soluble reducing agent and alkaline pH adjusting agent, wherein the water-soluble reducing agent is thiourea dioxide or sodium hydrosulfite, and the weight ratio of the water-soluble reducing agent to the alkaline pH adjusting agent is 1:0.3-1.3. The invention also includes a preparation method of heliotropin. The preparation method includes the steps as follows: adding water with weight equivalent to 0.5-5 times that of heliotropin in the heliotropin which is oxidized by nitrate oxidant; adding heliotropin decolorizer with mass concentration of 1-15%; stirring to uniform; heating to full reaction; standing for layering; removing supernatant and water-soluble reducing agent at the bottom layer; and fractionating residua to obtain heliotropin. With the method of the invention, the yield achieves above 85%; while the yield of white heliotropin crystals prepared with other methods is only 65%; and in the invention, the impurities are few, the appearance of the product is good (white crystal instead of faint yellow crystal), odour is intense, and no peculiar smell is generated.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to the synthesis technology of jasmonal. Background technique [0002] Jasmonal, also known as piperonal and heliotrope, has a chemical name of 3,4-methylenedioxybenzaldehyde, and its appearance is white or light yellow crystals. It has a sweet bean and fennel aroma, a perfume-like herb smell, and a cherry-like aroma. It is a floral fragrance with a light and long-lasting aroma. A small amount of its natural products are found in flower oils such as jasmine and black locust flowers and carnations. beans and other plants. It can be widely used in various daily cosmetic flavors and food flavors, and it is also widely used in spice processing, medicine, pesticide and electroplating industries. [0003] Now domestic jasmonal synthesis methods mainly include three methods: the synthesis of piperine as the raw material, the synthesis of isosafrole as the starting material and the synth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/54
Inventor 田长江
Owner 重庆德馨香料植物开发有限公司
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