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Method for synthesizing p-methoxybenzoic acid

A technology of methoxybenzoic acid and a synthesis method, applied in the field of synthesizing p-methoxybenzoic acid, can solve problems such as backward development of organic photochemistry, and achieve the effects of reducing reaction process costs, reducing costs, and reducing manufacturing costs

Inactive Publication Date: 2014-06-11
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But in China, the development of organic photochemistry is still relatively backward

Method used

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  • Method for synthesizing p-methoxybenzoic acid

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Effect test

Embodiment 1

[0023] In a 50 mL quartz reaction flask, add 41 mg (4-methoxybenzyl) trimethylsilane, 10 mL anhydrous acetonitrile, 5.4 μL hydrogen bromide solution (aq. 40%), magnetically in a pure oxygen environment Stirring, 25 oC Place the reaction flask under a 300W xenon lamp light source for 6 hours. According to the analysis of TLC and high performance liquid chromatography, the raw material (4-methoxybenzyl) trimethylsilane has been reacted completely, and only a single product is formed. Vacuum rotary evaporation, column chromatography separation and purification, the product is p-methoxybenzoic acid, the product mass is 29 mg, and the yield is 90%.

Embodiment 2

[0025] In a 50 mL quartz reaction flask, add 41 mg (4-methoxybenzyl) trimethylsilane, 10 mL anhydrous acetonitrile, 5.4 μL hydrogen bromide solution (aq. 40%), magnetically in a pure oxygen environment Stirring, 50 o Place the reaction flask under a 300W xenon lamp light source for 12 hours at C. After the reaction time is reached, the raw material (4-methoxybenzyl) trimethylsilane has been reacted completely and only a single product is formed by TLC and high performance liquid chromatography analysis. Vacuum rotary evaporation, separation and purification by column chromatography, the product is p-methoxybenzoic acid, the product mass is 26 mg, and the yield is 81%.

Embodiment 3

[0027] In a 50 mL quartz reaction flask, add 42 mg (4-methoxybenzyl) trimethylsilane, 10 mL anhydrous acetonitrile, 5.4 μL hydrogen bromide solution (aq. 40%), magnetically in a pure oxygen environment Stirring, 0 o Place the reaction flask under a 300W xenon lamp light source for 4 hours at C. After the reaction time is reached, the raw material (4-methoxybenzyl) trimethylsilane has been reacted completely and only a single product is formed by TLC and high performance liquid chromatography analysis. Vacuum rotary evaporation, column chromatography separation and purification, the product is p-methoxybenzoic acid, the product mass is 28 mg, and the yield is 85%.

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Abstract

The invention provides a method for synthesizing p-methoxybenzoic acid, which takes illumination of a xenon lamp as a condition, takes air or oxygen for oxidizing, and uses a hydrogen bromide water solution as a catalyst to synthesize the p-methoxybenzoic acid. The method for synthesizing the p-methoxybenzoic acid has outstanding advantages of taking illumination of the xenon lamp as an energy source, providing a completely new method for preparing various fine chemicals in industry, avoiding high toxic reagents and reagents easy to produce poison in traditional synthesis methods, improving cleanliness of industrial synthesis reaction, lowering environment contamination, being finished by one step, using single kind of raw materials, and improving the technological economical efficiency.

Description

[0001] 1. Technical field [0002] The invention relates to a method for synthesizing p-methoxybenzoic acid, in particular to a method for synthesizing p-methoxybenzoic acid under the conditions of xenon light irradiation, air or oxygen oxidation, and hydrogen bromide aqueous solution as a catalyst. [0003] 2. Background technology [0004] 4-methoxybenzoic acid (4-methoxybenzoic acid) is a colorless needle-like crystal at room temperature, with a melting point of 182~185 o C, the boiling point is 275 o C, the flash point is 185 oC , also known as p-anisic acid, 4-anisic acid, anisic acid, soluble in ethanol, ether, chloroform, slightly soluble in hot water, hardly soluble in cold water. p-Methoxybenzoic acid is an intermediate of many drugs and spices, for example, it is an intermediate of the new high-efficiency, low-toxicity intelligence-improving drug Inpiracetam, and an important intermediate of the antiarrhythmic drug Amiodarone. Can be used in fragrances and pre...

Claims

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Application Information

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IPC IPC(8): C07C65/21C07C51/265
CPCC07C51/255C07C65/21
Inventor 彭新华张亚成孙京
Owner NANJING UNIV OF SCI & TECH