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Synthesis method of p-nitrobenzoic acid

A technology of p-nitrobenzoic acid and synthesis method, which is applied in the field of synthesis of p-nitrobenzoic acid, can solve the problems of low product yield and purity, low reaction safety, and high equipment requirements, and achieve short reaction routes and high product purity. High effect with low equipment requirements

Inactive Publication Date: 2018-10-16
SICHUAN WUSHENG CHUNRUI MEDICAL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the synthesis method of p-nitrobenzoic acid is generally obtained by oxidation of p-nitrotoluene; the process of this method is relatively complicated, and the reaction needs to be carried out under relatively stable and certain pressure, which requires high equipment and relatively safe reaction. Low, and the yield and purity of the product are relatively low, it is necessary to improve

Method used

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  • Synthesis method of p-nitrobenzoic acid
  • Synthesis method of p-nitrobenzoic acid
  • Synthesis method of p-nitrobenzoic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Preparation of 2-p-nitrobenzoyl-2-acetamido-1,3-propanediol

[0023] The method is: first add 400kg of methanol, 420kg of 2-acetamido 4-nitroacetophenone, stir for 30 minutes, add dropwise 200kg of formaldehyde with a mass percentage of 37%, then add 0.5kg of sodium bicarbonate, and slowly heat to 35°C. Stop heating and control the reaction within 45°C, control the reaction sampling, cool to 5°C after the reaction is completed, centrifuge and filter to obtain 380kg of chloramphenicol intermediate, and then carry out vacuum distillation on the centrifuged mother liquor to recover methanol; after cooling to 10°C, centrifuge Promptly get 40kg of 2-p-nitrophenyl 2-acetylaminopropanediol product, and the mass percentage composition is 98.07%, and its content HPLC detection result is as follows figure 1 shown.

Embodiment 2

[0025] The synthetic method of p-nitrobenzoic acid:

[0026] Add 50 g of 2-p-nitrobenzoyl-2-acetylamino-1,3-propanediol prepared in Example 1 into a 500 ml three-neck flask, then add 190 g of water and 60 g of nitric acid, and slowly heat up to 100°C for reflux reaction 6 Hour, then cool to 20 ℃ of crystallizations with cooling water, filter to obtain p-nitrobenzoic acid 28.5 grams, yield 96.1%, content 99.5%, its content HPLC detection result is as follows: figure 2 shown.

Embodiment 3

[0028] The synthetic method of p-nitrobenzoic acid:

[0029] Put 50 g of 2-p-nitrobenzoyl-2-acetylamino-1,3-propanediol prepared in Example 1 into a 500 ml three-necked flask, then add 200 g of water and 65 g of nitric acid, and slowly heat up to 100°C for reflux reaction 6 Hours, then cooled to 20 ° C crystallization with cooling water, filtered to obtain 29 grams of p-nitrobenzoic acid, yield 97.8%, content 99.8%.

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Abstract

The invention discloses a synthesis method of p-nitrobenzoic acid. Reacting is performed by adopting 2-p-nitrobenzoyl-2-acetamino-1,3-propylene glycol and nitric acid as raw materials and water as a solvent; after the reacting, p-nitrobenzoic acid is obtained through crystallization. According to the method disclosed by the invention, the reaction conditions are mild, the reacting is performed atrelatively low temperature and under normal pressure, the requirements on equipment are low, the reaction line is short and thus the reacting is easy to control and safe and reliable; moreover, the obtained crude product has the advantages of easiness in separation, high yield and high purity and is suitable for popularization.

Description

[0001] Technical Field The present invention relates to the technical field of chemical synthesis, in particular to a synthetic method of p-nitrobenzoic acid. Background technique [0002] p-Nitrobenzoic acid is a yellow crystalline powder, odorless and capable of sublimation. Slightly soluble in water, soluble in organic solvents such as ethanol. Combustible in case of open flame and high heat; decomposes when heated. p-Nitrobenzoic acid is mainly used as an intermediate in organic synthesis such as medicine, dye, veterinary drug, and photosensitive material. Used in the production of procaine hydrochloride, procainamide hydrochloride, p-aminomethylbenzoic acid, folic acid, benzocaine, cough, cephalosporin V, p-aminobenzoyl glutamic acid, shellfish Nier, as well as the production of reactive brilliant red M-8B, reactive red violet X-2R and light filters, color film couplers, metal surface rust removers, sunscreens, etc. The average annual growth rate of China's vanillin exp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C205/57C07C231/12C07C233/18
CPCC07C201/12C07C231/12C07C205/57C07C233/31C07C233/18
Inventor 朱泽文胡奎赵勇郭小刚黄瑜周刘阳
Owner SICHUAN WUSHENG CHUNRUI MEDICAL CHEM
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