Synthetic method for mint benzoate

A synthesis method and technology of benzoic acid, which are applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve problems such as corrosion, environmental pollution, troublesome operation, etc., and achieve high ester yield and high synthesis process. Simple, high-value effects

Inactive Publication Date: 2014-02-19
太仓市运通化工厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually esterification under the catalysis of sulfuric acid, the above reaction has environmental pollution and serious corrosion, and some operations are troublesome and costly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] In a 1000mL three-necked flask equipped with a stirrer, a thermometer and a reflux condenser with a water separator, add 156g of menthol, 97.6g of benzoic acid and 2.5g of p-toluenesulfonic acid catalyst, heat and reflux to control the temperature at 95 ~102°C, time when there is reflux, and react for 10 hours. After the reaction is over, wash the cooled solution with deionized water and sodium carbonate solution, separate the liquids, dry with anhydrous magnesium carbonate, and filter out the magnesium sulfate after drying. Obtain clear light yellow solution, carry out normal pressure distillation with solution, evaporate cyclohexane when 81 ℃, carry out vacuum distillation with menthyl benzoate crude product, collect 263~271 ℃ (5.8kPa) cut as product, produce The rate is 65.3%.

Embodiment 2

[0014] In a 1000mL three-necked flask equipped with a stirrer, a thermometer and a reflux condenser with a water separator, add 156g of menthol, 195.2g of benzoic acid and 14g of p-toluenesulfonic acid catalyst, heat and reflux to control the temperature at 95- 102°C, time when there is reflux, and react for 2 hours. After the reaction is over, wash the cooled solution with deionized water and sodium carbonate solution, separate the liquids, dry with anhydrous magnesium carbonate, and filter out the magnesium sulfate after drying to obtain Clarify the light yellow solution, distill the solution at atmospheric pressure, distill off the cyclohexane at 81°C, carry out vacuum distillation on the crude menthyl benzoate product, collect the distillate at 263~271°C (5.8kPa) as the product, the yield 72.6%.

Embodiment 3

[0016] In the 1000mL there-necked flask equipped with a stirrer, a thermometer and a reflux condenser with a water separator, add 156g of menthol, 170.8g of benzoic acid and 9.8g of p-toluenesulfonic acid catalyst, and heat and reflux to control the temperature at 95 ~102°C, time when there is reflux, and react for 8 hours. After the reaction is over, wash the cooled solution with deionized water and sodium carbonate solution, separate the liquids, dry with anhydrous magnesium carbonate, and filter out the magnesium sulfate after drying. Obtain clear light yellow solution, carry out normal pressure distillation with solution, evaporate cyclohexane when 81 ℃, carry out vacuum distillation with menthyl benzoate crude product, collect 263~271 ℃ (5.8kPa) cut as product, produce The rate is 80.2%.

[0017] Compared with the synthetic method of traditional menthyl benzoate, p-toluenesulfonic acid is a good catalyst for the synthesis of menthyl benzoate, has higher practical applicat...

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PUM

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Abstract

The invention discloses a synthetic method for mint benzoate. The method comprises the following steps: adding menthol and benzoic acid according to a mol ratio of 1: 0.8-1.6 and adding the catalyst para-toluenesulfonic acid accounting for 1 to 4% of the weight of menthol and benzoic acid; carrying out heating reflux at a temperature of 95 to 102 DEG C, beginning timing when reflux appears and allowing a reaction to last for 2 to 10 h; after completion of the reaction, successively subjecting a cooled solution to washing with deionized water, washing with a sodium carbonate solution and liquid separation; carrying out drying by using anhydrous magnesium carbonate and removing magnesium sulfate through filtration after drying so as to obtain a clear light-yellow solution; and subjecting the solution to normal pressure distillation, removing cyclohexane through steaming at a temperature of 81 DEG C, subjecting a crude mint benzoate product to reduced pressure distillation and collecting a fraction obtained at 263 to 271 DEG C (5.8 kPa) as a product. According to the invention, para-toluenesulfonic acid is a good catalyst for synthesis of mint benzoate, and the synthetic method has the advantages of a high practical application value, high yield of mint benzoate and simple synthesis process.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a synthetic method of menthyl benzoate. Background technique [0002] Menthyl benzoate is a light yellow transparent liquid with a cool mint taste. It is an important compound and is used as a fixative in the deployment of daily chemical essences. It is mainly used in industry and daily chemical industry. It is a high-grade spice that needs to be developed and has a bright future. Usually, the esterification is carried out under the catalysis of sulfuric acid. The above reaction has environmental pollution and serious corrosion, and some operations are troublesome and the cost is high. In order to overcome the above deficiencies, once someone tried to find different catalysts to catalyze the synthesis of isoamyl benzoate. As a strong organic acid, p-toluenesulfonic acid has less side reactions than sulfuric acid, and is cheap and easy to obtain. Contents ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/78C07C67/08
CPCC07C67/08
Inventor 张卫东
Owner 太仓市运通化工厂
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