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Preparation method of 1,2,3-trimethoxy-5-allylbenzene

A technology of trimethoxybenzene and allylbenzene, which is applied in the direction of ether preparation, ester reaction to prepare ether, isomerization to prepare ether, etc., can solve the problems of difficult industrial mass production, high cost, and few reaction steps, and achieve The effect of low price, low cost and low production cost

Inactive Publication Date: 2014-12-24
程文峰
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The advantage of this route method is that the number of reaction steps is small, and the disadvantage is that column chromatography is used, the cost is high, it is difficult to carry out industrial mass production, and the total yield is only 25.8%.

Method used

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  • Preparation method of 1,2,3-trimethoxy-5-allylbenzene
  • Preparation method of 1,2,3-trimethoxy-5-allylbenzene
  • Preparation method of 1,2,3-trimethoxy-5-allylbenzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Step a: Add 126 g of pyrogallic acid, 300 g of water and stir in the reaction bottle, 328 ml of 30% liquid caustic soda, add 310 ml of dimethyl sulfate dropwise at about 40°C, and the internal temperature of the reaction should not exceed 60°C, pH≥9. After the dropwise addition, heat up to 90°C and keep it warm for 1 hour, cool, separate the liquid, extract the precipitated solid with toluene in the water layer, filter and separate it, then distill it under reduced pressure, collect the fraction at 130-132°C (20mmHg), and obtain a white crystalline solid with a yield of 90%. .

[0038] Step b: Add 800ml of dichloromethane and 400g of aluminum trichloride to the reaction bottle, and dropwise add a dichloromethane solution of 1,2,3-trimethoxybenzene under stirring (168g of 1,2,3-trimethoxybenzene dissolves In 200ml of dichloromethane), the temperature is controlled at 20-40°C during the dropwise addition, and the stirring is continued for 2-3 hours after the dropwise add...

Embodiment 2

[0043] The selective demethylation reagent of step b is changed to AlCl 3 , other conditions are reacted under the same conditions as in Example 1, and the results are shown in Table 1.

Embodiment 3

[0045] The selective demethylation reagent in step b was changed to methanesulfonic acid, and the reaction was carried out under the same conditions as in Example 1, and the results are shown in Table 1.

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Abstract

The invention provides a preparation method of 1,2,3-trimethoxy-5-allylbenzene. The synthetic route of the preparation method is as shown in the specification. According to the preparation method disclosed by the invention, the synthetic process conditions are simple, the cost is low, the total yield of the reaction can be above 49% and the preparation method is suitable for industrialized mass production and has significant business values.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for preparing 1,2,3-trimethoxy-5-allylbenzene. Background technique [0002] In the process of grain storage, in order to control pests and protect the quality of grain, it is often necessary to use pesticides. However, long-term and continuous use of large amounts of chemical insecticides that are highly toxic to humans will not only cause pests to develop resistance to pesticides to varying degrees, but also cause serious environmental pollution and damage human health and ecological safety. New insecticides with high efficiency, low toxicity, no pollution, and less resistance to pesticides have become an inevitable trend. Due to the high biological activity to stored grain pests, not easy to produce drug resistance, low toxicity to humans and animals, and no pollution to the environment, natural medicinal plants have increasingly great potential to replace non-natur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/215C07C41/16
CPCC07C41/01C07C41/16C07C41/26C07C41/32C07C43/215C07C43/23C07C43/2055
Inventor 程文峰徐晓东
Owner 程文峰
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