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A kind of synthetic method of methyl 3,4,5-trimethoxybenzoate

A technology of methyl trimethoxybenzoate and trimethoxybenzoic acid, which is applied in the field of chemistry, can solve problems such as incomplete reaction, achieve the effects of complete reaction of raw materials, reduce production costs, and reduce waste

Active Publication Date: 2018-11-23
JIURUI BIOLOGY & CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] For the problems referred to above, the object of the present invention provides a kind of synthetic method of 3,4,5-trimethoxymethyl benzoate, it carries out esterification reaction with methyl chloride as reactant, not only solves the incomplete reaction problem in the traditional technique problems, and greatly reduces the degree of danger in production operations

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  • A kind of synthetic method of methyl 3,4,5-trimethoxybenzoate
  • A kind of synthetic method of methyl 3,4,5-trimethoxybenzoate

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Embodiment 1: a kind of synthetic method of 3,4,5-trimethoxymethylbenzoate, concrete method and step are:

[0026] (1) Add 20g of 3,4,5-trimethoxybenzoic acid, 80ml of DMF, 4g of sodium hydroxide, and 2g of sodium bromide into a three-necked flask, stir, cool down to below 10°C, and inject 6g of methyl chloride gas. After passing through, the temperature was raised to about 45°C, and the reaction was kept for 5 hours;

[0027] (2) After the reaction is completed, distill and concentrate, add the concentrated solution to 200ml of experimental water, stir and cool down to room temperature, let stand, precipitate and then suction filter to obtain the crude product;

[0028] (3) Put the crude product into 80ml of methanol, stir and heat up to 60-65°C, reflux for 1 hour and then cool down to room temperature. After concentrated distillation, suction filtration and drying, 18.2g of pure product was obtained, the yield was about 85.4%, the content was 99.89% by HPLC, and the ...

Embodiment 2

[0029] Embodiment 2: a kind of synthetic method of 3,4,5-trimethoxymethylbenzoate, concrete method and step are:

[0030] (1) Add 20g of 3,4,5-trimethoxybenzoic acid, 150ml of DMF, 5g of sodium carbonate, and 3g of sodium bromide into a three-neck flask, stir, cool down to below 10°C, and inject 6g of methyl chloride gas. After passing through, the temperature was raised to about 50°C, and the heat preservation reaction was carried out for 4 hours;

[0031] (2) After the reaction is completed, distill and concentrate, add the concentrated solution to 300ml of experimental water, stir and cool down to room temperature, let stand, precipitate and then suction filter to obtain the crude product;

[0032] (3) Put the crude product into 60ml of methanol, stir and heat up to 60-65°C, reflux for 1 hour and then cool down to room temperature. After concentrated distillation, suction filtration and drying, 18.0 g of pure product was obtained, the yield was about 84.5%, the content was...

Embodiment 3

[0033] Embodiment 3: a kind of synthetic method of 3,4,5-trimethoxymethylbenzoate, concrete method and step are:

[0034] (1) Add 60g of 3,4,5-trimethoxybenzoic acid, 300ml of DMF, 18g of sodium carbonate, and 12g of sodium bromide into a three-necked flask, stir, cool down to below 10°C, and inject 18g of methyl chloride gas. After passing through, the temperature is raised to about 55°C, and the reaction is kept for 3 hours;

[0035] (2) After the reaction is completed, distill and concentrate, add the concentrated solution to 700ml of experimental water, stir and cool down to room temperature, let stand, precipitate and then suction filter to obtain the crude product;

[0036] (3) Put the crude product into 220ml of methanol, stir and heat up to 60-65°C, reflux for 1 hour and then cool down to room temperature. After concentrated distillation, suction filtration and drying, 54.1 g of pure product was obtained, the yield was about 84.7%, the content was 99.63% by HPLC, and ...

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Abstract

The invention discloses a synthesis method for 3,4,5-trimethoxybenzoate. According to the synthesis method, 3,4,5-trimethoxybenzoic acid serves as a raw material, N,N-dimethylformamide serves as solvent, 3,4,5-trimethoxybenzoic acid and N,N-dimethylformamide are subjected to an esterification reaction with chloromethane gas at the temperature of 20 DEG C-60 DEG C, in the reaction process, any one inorganic alkaline compound of potassium carbonate, sodium carbonate, potassium hydroxide and sodium hydroxide serves as an acid binding agent, whether a catalyst is added or not is determined according to the specific reaction condition, and any one or a mixture of polyethylene glycol and sodium bromide serves as the catalyst. The method is simple and practicable, easy and convenient to operate, efficient and environmentally friendly and can be used for commercialized scale production to meet the ever-increasing market requirements.

Description

technical field [0001] The invention belongs to the technical field of chemistry, in particular to a method for synthesizing methyl 3,4,5-trimethoxybenzoate. technical background [0002] 3,4,5-Methyl trimethoxybenzoate, a white crystalline solid, is an important intermediate in organic synthesis. Starting from this substance, a variety of pharmaceutical products can be obtained, such as antibacterial synergistic drug trimethoprim, anxiolytic drug trimetazine, gastrointestinal drug trimebutine maleate, etc., and can also be used in heat-sensitive recording materials Used as a UV absorber. With the continuous development of the chemical industry, 3,4,5-trimethoxymethylbenzoate has a broader market prospect. Therefore, it is possible to produce 3,4,5-trimethoxymethylbenzoate simply and efficiently There are great social benefits. [0003] At present, the preparation method commonly used in industry is obtained by esterifying 3,4,5,-trimethoxybenzoic acid with methanol under...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/92C07C67/10
CPCC07C67/10C07C67/54C07C67/56C07C69/92
Inventor 杨彦明陈波王文龙赵国锋
Owner JIURUI BIOLOGY & CHEM CO LTD
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