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Preparation method for benzoic acid

A technology of benzoic acid and benzophenone, which is applied in the field of preparation of benzoic acid, can solve the problems of backward development of organic photochemistry, etc., and achieve the effects of reducing the cost of the reaction process, improving cleanliness, and reducing energy consumption

Inactive Publication Date: 2014-07-09
FUDAN UNIV
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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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  • Preparation method for benzoic acid
  • Preparation method for benzoic acid
  • Preparation method for benzoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 50 mL quartz reaction vial, add 92 mg toluene, 10 mL solvent acetonitrile, 5 mg benzophenone, magnetically stir in air atmosphere, at 25 o C temperature, Xe lamp (300 W) under light for 10 hours. After the reaction time was up, only a single product, benzoic acid, was generated through high-performance liquid chromatography analysis. Rotary evaporation in vacuum, separation and purification by column chromatography, the product quality is 51 mg, and the yield rate is 42%, [ 1 H NMR (400 MHz, CDCl 3 ): δ 12.26 (brs, 1 H), 8.13 (d, J = 8.0 Hz, 2 H), 7.65-7.55 (m, 1 H), 7.54-7.30 (m, 2 H)]. Keeping other conditions unchanged, change the temperature of the above reaction, respectively at 0 o C, 50 o Carried out at C temperature, temperature increase or decrease all make the productive rate of this reaction reduce.

Embodiment 2

[0026] In a 50 mL quartz reaction flask, add 92 mg toluene, 10 mL solvent acetonitrile, 10 mg benzophenone, magnetically stir in the air atmosphere, at 25 o C temperature, under the light of Xe lamp (300 W) for 6 hours. After the reaction time was up, only a single product, benzoic acid, was generated through high-performance liquid chromatography analysis. Rotary evaporation in vacuum, separation and purification by column chromatography, the product quality is 82 mg, and the yield is 67%. Keeping other conditions unchanged, change the temperature of the above reaction, respectively at 0 o C, 50 o Carried out at C temperature, temperature increase or decrease all make the productive rate of this reaction reduce.

Embodiment 3

[0028] In a 50 mL quartz reaction vial, add 92 mg toluene, 10 mL solvent acetonitrile, 20 mg benzophenone, magnetically stir in air atmosphere, at 25 o C temperature, under the light of Xe lamp (300 W) for 3 hours. After the reaction time was up, only a single product, benzoic acid, was generated through high-performance liquid chromatography analysis. Rotary evaporation in vacuum, separation and purification by column chromatography, the product quality is 120 mg, and the yield is 98%. Keeping other conditions unchanged, change the temperature of the above reaction, respectively at 0 o C, 50 o Carried out at C temperature, temperature increase or decrease all make the productive rate of this reaction reduce.

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Abstract

The invention relates to a preparation method for benzoic acid. The preparation method comprises the following concrete steps: adding toluene into a reactor; carrying out a reaction under magnetic stirring at a temperature of 25 DEG C in air an atmosphere; and carrying out a full reaction under 300 W Xelamp illumination conditions so as to obtain desired benzoic acid. The method provided by the invention avoids usage of reagents with high corrosivity, high toxicity and easy production of toxicity used in traditional synthetic methods, improves cleanness of an industrial synthesis reaction and reduces environmental pollution and energy consumption. Benzophenone is used as a reaction catalyst in the method, so cost is decreased. The method is completed in one step and uses a single kind of raw material, so the method has improved process economical efficiency.

Description

technical field [0001] The present invention relates to a kind of method of preparing benzoic acid, especially a kind of preparation method of benzoic acid. Background technique [0002] Benzoic acid is scaly or needle-like crystals with the smell of benzene or formaldehyde. Melting point 122.13 o C, boiling point 249 o C, Slightly soluble in water, easily soluble in organic solvents such as ethanol and ether. Benzoic acid is used in the production of medicines, dye carriers, plasticizers, spices and food preservatives, and is also used in the performance improvement of alkyd resin coatings. Benzoic acid is an important acid-type food preservative. Its molecular formula is C 7 h 6 o 2 , the relative molecular mass is 122.1214. The structural formula of benzoic acid is: [0003] [0004] At present, the production process of preparing benzoic acid by thermal oxidation of toluene is widely used in the world. The method utilizes heavy metal salt cobalt or manganese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/06C07C51/265
CPCC07C51/265C07C63/06
Inventor 郭浩胡建华
Owner FUDAN UNIV
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