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Preparation process of ethyl p-nitrobenzoate

A technology of ethyl nitrobenzoate and p-nitrobenzoic acid, applied in the field of preparation of ethyl p-nitrobenzoate, achieving good application prospects, improving production efficiency, and avoiding complicated operations

Inactive Publication Date: 2019-08-02
常州瑞曦生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by this invention is to overcome the defective of prior art, improve a kind of preparation technology of p-nitrobenzoic acid ethyl ester, its technology is simple, pollution-free, efficient height, safety height, improved p-nitrobenzoate by this technology Purity and conversion of ethyl benzoate

Method used

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  • Preparation process of ethyl p-nitrobenzoate
  • Preparation process of ethyl p-nitrobenzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Get 22.4g p-nitrobenzoic acid and be dissolved in ethanol solution (mass percentage composition of ethanol is 99.9%), be configured into the p-nitrobenzoic acid solution that percentage composition is 4%, put into feed tank circulation, in The sulfonic acid resin catalyst is filled in the fixed-bed catalytic micro-reaction tank, the temperature of the feed tank is set to 70°C, the temperature of the fixed-bed catalytic micro-reaction tank is 80°C, the reaction pressure is 0.4MPa, and the flow rate is 5ml / min. Turn on the liquid phase pump, inject the solution in the feed tank into the fixed bed catalytic micro-reaction tank, and then receive the liquid out. In the continuous reaction, three product samples and one mixed sample were taken and detected by high performance liquid chromatography, and the conversion rate of the reaction was 89.92%.

Embodiment 2

[0043] Get 22.4g p-nitrobenzoic acid and dissolve in ethanol solution (mass percentage composition of ethanol is 99.9%), configure the p-nitrobenzoic acid solution that percentage composition is 4%, put into feed tank and circulate. Fill the sulfonic acid resin catalyst in the fixed-bed catalytic micro-reaction tank, set the temperature of the feed tank to 70°C, the temperature of the fixed-bed catalytic micro-reaction tank to 80°C, the reaction pressure to 0.4MPa, and the flow rate to 10ml / min. Turn on the liquid phase pump, inject the solution into the fixed-bed catalytic micro-reaction tank, and receive the effluent. In the continuous reaction, three product samples and one mixed sample were taken and detected by high-performance liquid chromatography, and the conversion rate of the reaction was 86.55%.

Embodiment 3

[0045] Get 22.4g p-nitrobenzoic acid and dissolve in ethanol solution (mass percentage composition of ethanol is 99.9%), configure the p-nitrobenzoic acid solution that percentage composition is 4%, put into feed tank and circulate. Fill the sulfonic acid resin catalyst in the fixed-bed catalytic micro-reaction tank, set the temperature of the feed tank to 70°C, the temperature of the fixed-bed catalytic micro-reaction tank to 80°C, the reaction pressure to 0.4MPa, and the flow rate to 20ml / min. Turn on the liquid phase pump, inject the solution into the fixed-bed catalytic micro-reaction tank, and receive the effluent. In the continuous reaction, three product samples and one mixed sample were taken and detected by high performance liquid chromatography, and the conversion rate of the reaction was 81.41%.

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Abstract

The invention discloses a preparation process of ethyl p-nitrobenzoate. The method comprises steps as follows: ethanol is taken as a solvent, and a p-nitrobenzoic acid solution is prepared; the p-nitrobenzoic acid solution is put in a feeding tank and pumped into a fixed bed catalytic microreaction tank through a liquid phase pump, an esterification reaction is performed under the action of a catalyst in the fixed bed catalytic microreaction tank, and an obtained product is treated to obtain ethyl p-nitrobenzoate. The process is simple, pollution-free and high in efficiency and safety, and thepurity and the conversion rate of ethyl p-nitrobenzoate are increased with the process.

Description

technical field [0001] The invention relates to a preparation process of ethyl p-nitrobenzoate. Background technique [0002] Currently, ethyl p-nitrobenzoate is a chemical substance with the formula C 9 h 9 NO 4 . Colorless or light yellow needle crystal. The melting point is 57°C and the boiling point is 186.3°C. Soluble in ethanol and ether, insoluble in water. It is mainly used as an intermediate in organic synthesis. In the pharmaceutical industry, it is used in the production of local anesthetics such as benzocaine, tetracaine hydrochloride and cough suppressants. Benzocaine (ABEE) is also known as ethyl aminobenzoate. Colorless orthorhombic crystal, odorless and tasteless. Molecular weight 165.19. The melting point is 91-92°C. Soluble in alcohol, ether, chloroform. Soluble in almond oil, olive oil, dilute acid. Insoluble in water. It is clinically used for pain relief and antipruritic of wounds, ulcers, burns, skin abrasions and hemorrhoids. Local appli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/57C07C201/12
CPCC07C201/12C07C205/57
Inventor 朱子轩
Owner 常州瑞曦生物科技有限公司
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