Synthesis method of heliotropin

A synthetic method, piperonal aldehyde technology, applied in the field of piperonal aldehyde synthesis, can solve problems such as troublesome environmental pollution, hidden dangers of hydrogen peroxide safety, explosion, etc., and achieve the effect of improving product quality, solving corrosion problems, and reducing corrosion

Active Publication Date: 2021-07-27
BROTHER ENTERPRISES HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the existing related oxidation methods, the patent number: CN 01804348.8 uses nitric acid as an oxidant, and the product has nitrification by-products that are difficult to separate, which affects product quality and causes troublesome environmental pollution.
Patent No.: CN 103923056 B uses hydrogen peroxide as an oxidant, but hydrogen peroxide has potential safety hazards during industrial use, and explosion accidents sometimes occur

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A synthetic method of piperonal, the specific steps of the method are as follows:

[0024] Add 29.6kg of 50% (wt) glyoxylic acid aqueous solution to a 200L enamel reaction kettle, cool down to 0°C, add 48kg of 98% (wt) sulfuric acid aqueous solution, and 24.4kg of catechol methylene ether, and control the reaction temperature at 0-20°C , continue to react for 24-48h, add 48.8kg of water to terminate the reaction if the central control is qualified; press filter, separate the water phase, add the solid to a 500L enamel reaction kettle, then add 22kg of 30% (wt) hydrochloric acid, 100kg of toluene, and 3.2kg of catalyst cobalt sulfate , be warmed up to 80 ℃ and start to add 10% (wt) sodium percarbonate aqueous solution (150kg) dropwise, react for 1-4h, pass the central control and drop to room temperature, stop stirring, stand for phase separation, separate the water phase to recover the catalyst, and the oil phase Wash once with 20 kg of aqueous sodium hydroxide solution...

Embodiment 2

[0027] Add 29.6kg of 50% (wt) glyoxylic acid aqueous solution to a 200L enamel reaction kettle, cool down to 0°C, add 48kg of 98% (wt) sulfuric acid aqueous solution, and 24.4kg of catechol methylene ether, and control the reaction temperature at 0-20°C , continue to react for 24-48h, add 48.8kg of water to terminate the reaction if the central control is qualified; press filter, separate the water phase, add the solid to a 500L enamel reactor, then add 22kg of 30% (wt) hydrochloric acid, 100kg of toluene, and 2.7kg of catalyst cobalt chloride kg, be warmed up to 80°C and start to add 10% (wt) sodium percarbonate aqueous solution (150kg) dropwise, react for 1-4h, pass the central control and drop to room temperature, stop stirring, let stand to separate the phases, separate the water phase to recover the catalyst, oil The phases are washed once with 20 kg of aqueous sodium hydroxide solution and 48 kg of water with a mass fraction of 5%, respectively. After washing, the oil pha...

Embodiment 3

[0033] Add 29.6kg of 50% (wt) glyoxylic acid aqueous solution to a 200L enamel reaction kettle, cool down to 0°C, add 48kg of 98% (wt) sulfuric acid aqueous solution, and 24.4kg of catechol methylene ether, and control the reaction temperature at 0-20°C , continue to react for 24-48h, add 48.8kg of water to stop the reaction if the central control is qualified; press filter, separate the water phase, add the solid to a 500L enamel reactor, then add 22kg of 30% (wt) hydrochloric acid, 100kg of chloroform, and 3.2kg of catalyst cobalt sulfate , be warmed up to 80 ℃ and start to add 10% (wt) sodium percarbonate aqueous solution (150kg) dropwise, react for 1-4h, pass the central control and drop to room temperature, stop stirring, stand for phase separation, separate the water phase to recover the catalyst, and the oil phase Wash once with 20 kg of aqueous sodium hydroxide solution and 48 kg of water with a mass fraction of 5%, respectively. After washing, the oil phase enters a re...

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Abstract

The invention relates to a synthesis method of heliotropin, and belongs to the technical field of chemical synthesis. According to the synthesis method of heliotropin, an intermediate piperonyl glycollic acid prepared by taking catechol methylene ether as a raw material is taken as a raw material, cobalt salt is taken as a catalyst, sodium percarbonate is taken as an oxidizing agent, and the piperonyl glycollic acid is oxidized and decarboxylated in an acidic environment to synthesize the piperonal. In the experiment process, sodium percarbonate is adopted to replace hydrogen peroxide commonly used in heliotropin synthesis to serve as the oxidizing agent, it is accidentally found that a good effect is achieved, the raw material conversion rate can reach 99% or above, and the product yield can reach 92.4% or above. And the safe oxidizing agent sodium percarbonate is selected, so that the safety or environmental protection problem caused by using hydrogen peroxide or nitric acid is effectively avoided.

Description

technical field [0001] The invention relates to a synthesis method of piperonal, which belongs to the technical field of chemical synthesis. Background technique [0002] 3,4-Methylenedioxybenzaldehyde, referred to as piperonal, is a white or yellowish-white flashing crystal, which turns reddish brown when exposed to light in the air. Sweet vanilla and cherry-like aroma. The melting point is 37°C and the boiling point is 264°C. Very soluble in ethanol and ether, soluble in propylene glycol and most non-volatile oils, slightly soluble in mineral oil, insoluble in glycerin and water. [0003] In the prior art, piperonal is synthesized from catechol methylene ether as a raw material, first to obtain piperonyl glycolic acid, and then to obtain piperonal through oxidative decarboxylation. Among the existing related oxidation methods, the patent number: CN 01804348.8 uses nitric acid as the oxidant, and the product has nitrification by-products that are difficult to separate, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/54
CPCC07D317/54
Inventor 沈超倪宏亮吴小乐周中平
Owner BROTHER ENTERPRISES HLDG CO LTD
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