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Synthetic method of benzyl benzoate

A technology of benzyl benzoate and a synthesis method, applied in the synthesis field of benzyl benzoate, can solve problems such as high reaction temperature, large catalyst, high production cost, achieve high reaction conversion rate and selectivity, reduce production cost, The effect of low production cost

Inactive Publication Date: 2018-05-18
CHANGZHOU VOCATIONAL INST OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method needs to use zirconium dioxide and chromium trioxide as raw materials to prepare catalysts. The preparation process is complicated and the reaction steps are long, resulting in high production costs.
Chinese patent 102219662 discloses a kind of method for preparing benzyl benzoate with benzoic acid and toluene gas mixture as raw material, the catalyst of this method is made up of the composite oxide of Zr, Cu, Al, Zn, B and rare earth element, the preparation catalyst Raw materials are expensive and the preparation process is complicated
This method requires a large amount of catalyst, and the reaction time is longer and the reaction temperature is higher

Method used

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  • Synthetic method of benzyl benzoate
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  • Synthetic method of benzyl benzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A method for synthesizing benzyl benzoate through uncatalyzed esterification: 67.17g (550mmol) sodium benzoate, 63.29g (500mmol) benzyl chloride, 200mL N,N‐dimethylformamide are added in a three-necked flask, and heated at 80°C The next reaction. The reaction system was white and turbid at the beginning, and the reaction solution gradually became clear as the heating and stirring proceeded. Keep the reaction at 80°C. As the reaction progresses, white sodium chloride solids precipitate out in the reaction solution, and the reaction ends after 1.5 hours. After the reaction solution was cooled to room temperature, the Buchner funnel was suction-filtered, and the filtrate was collected. After distillation under reduced pressure, the solvent N, N-dimethylformamide was distilled off and the solution was in a white milky state. The separated sodium benzoate solid is separated by filtration, and the filtrate is removed by distillation and rectification to remove low-boilers a...

Embodiment 2

[0025] A method for synthesizing benzyl benzoate through uncatalyzed esterification: 91.59g (750mmol) sodium benzoate, 63.29g (500mmol) benzyl chloride, and 300mL toluene are added in a three-necked flask and reacted at 90°C. The reaction system was white and turbid at the beginning, and the reaction solution gradually became clear as the heating and stirring proceeded. The reaction was kept at 90°C. As the reaction progressed, white sodium chloride solids precipitated out in the reaction solution, and the reaction ended after 1 hour. After the reaction solution was cooled to room temperature, the Buchner funnel was suction-filtered, and the filtrate was collected. Distilled under reduced pressure, after the solvent toluene was distilled off, the solution was in a white milky state. The separated sodium benzoate solid is separated by filtration, and the filtrate is removed by distillation and rectification to remove low-boilers and high-boilers in the product to obtain the fi...

Embodiment 3

[0027] A method for synthesizing benzyl benzoate through uncatalyzed esterification: 109.91g (900mmol) sodium benzoate, 75.94g (600mmol) benzyl chloride, and 500mL chloroform are added in a three-necked flask, heated to reflux. The reaction system was white and turbid at the beginning, and the reaction solution gradually became clear as the heating and stirring proceeded. Keep reflux, along with the progress of the reaction, there is white sodium chloride solid to separate out in the reaction solution, and the reaction ends after 2 hours. After the reaction solution was cooled to room temperature, the Buchner funnel was suction-filtered, and the filtrate was collected. Distilled under reduced pressure, the solvent chloroform was distilled off, and the solution was in a white milky state. The separated sodium benzoate solid is separated by filtration, and the filtrate is removed by distillation and rectification to remove low-boilers and high-boilers in the product to obtain t...

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Abstract

The invention discloses a synthetic method of benzyl benzoate and belongs to the field of organic synthesis. The synthetic method comprises the following steps of adding sodium benzoate, benzyl chloride and a solvent in a reaction vessel, and performing reaction under the environment with the temperature of 60-100 DEG C to produce the benzyl benzoate; after reaction is finished, performing cooling, filtering the cooled benzyl benzoate to remove sodium chloride solids which precipitate from a reaction solution; after removing the solvent from the reaction solution with steaming, filtering excess sodium benzoate; removing low-boiling substances and high-boiling substances in a product from a filtrate solution through distillation and rectification to obtain a finished product. By avoiding use of a catalyst, the method is short in reaction time, simple in reaction condition and high in product yield.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to the synthetic method of benzyl benzoate Background technique [0002] Benzyl benzoate, also known as benzyl benzoate, is a colorless or pale yellow oily liquid with a light almond-like aroma. Benzyl benzoate is often used as a setting agent and flavoring agent for floral flavors, and is also widely used in food flavors. The product is also widely used as a plasticizer or solvent, especially when nitrocellulose is mixed with resin, it can be mixed with diethyl benzoate or dibutyl ester. In addition, the product can be used to prepare whooping cough medicine and asthma medicine, has the effect of dilating blood vessels and relieving spasm, and can be used as a raw material for compound progesterone acetate and mosquito repellent oil. [0003] There are several methods for the synthesis of benzyl benzoate. One is to use benzoic acid and benzyl alcohol as raw materials to obtain be...

Claims

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Application Information

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IPC IPC(8): C07C67/11C07C67/52C07C67/48C07C69/78
CPCC07C67/11C07C67/48C07C67/52C07C69/78
Inventor 吴东恩郭庆会李雪莲罗洋辉
Owner CHANGZHOU VOCATIONAL INST OF ENG
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