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Preparation method of ethopabate

A technology of ethopabate and methyl acetylaminosalicylate, which is applied in the field of chemical drug synthesis, can solve the problems of not being green and environmentally friendly, and achieve the effects of environmental friendliness, high yield, and resource saving

Inactive Publication Date: 2018-01-05
XUCHANG HENGSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is a large amount of strong acid-base wastewater in the process, which is not environmentally friendly

Method used

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  • Preparation method of ethopabate
  • Preparation method of ethopabate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Put (100.0g, 0.67mol) p-aminosalicylic acid and 5.0g p-toluenesulfonic acid in a 2L three-necked flask, add 500g methanol and stir evenly, raise the temperature to 65°C, and keep warm at 60-65°C for 4 hours. A reaction solution of methyl p-aminosalicylate was obtained.

[0020] Add (115.7g, 0.85mol) sodium acetate trihydrate to the reaction solution of methyl p-aminosalicylate, use 10% sodium carbonate or 10% acetic acid to control the pH range of the reaction solution to be 6.5-7.5, and control the temperature at 35- At 40°C, add 20.0 g of acetylase, strictly control the temperature and pH, react for 3 hours, and the reaction is complete. Methanol was recovered under reduced pressure, 500g of ethyl acetate was added to the mother liquor for extraction, liquid separation, drying and concentration were carried out, and then after cooling down and crystallization, suction filtration, and blast drying at 50°C, 196.7g of methyl p-acetylaminosalicylate was obtained. Yield 9...

Embodiment 2

[0023] Put (100.0g, 0.67mol) p-aminosalicylic acid and 8.0g p-toluenesulfonic acid in a 2L three-necked flask, add 800g methanol and stir evenly, raise the temperature to 65°C, and keep warm at 60-65°C for 3 hours. A reaction solution of methyl p-aminosalicylate was obtained.

[0024] Add (136.8g, 1.0mol) sodium acetate trihydrate to the reaction solution of methyl p-aminosalicylate, use 10% sodium carbonate or 10% acetic acid to control the pH range of the reaction solution to be 6.5-7.5, and control the temperature at 35- Add 40.0 g of acetylase at 40°C, strictly control the temperature and pH, react for 2 hours, and the reaction is complete. Methanol was recovered under reduced pressure, 500g of ethyl acetate was added to the mother liquor for extraction, liquid separation, drying and concentration were carried out, and then after cooling down and crystallization, suction filtration, and blast drying at 50°C, 199.2g of methyl p-acetylaminosalicylate was obtained. Yield 95....

Embodiment 3

[0027] Put (100.0g, 0.67mol) p-aminosalicylic acid and 10.0g p-toluenesulfonic acid in a 2L three-necked flask, add 600g methanol and stir evenly, raise the temperature to 65°C, keep warm at 60-65°C for 2 hours, A reaction solution of methyl p-aminosalicylate was obtained.

[0028] Add (115.7g, 0.85mol) sodium acetate trihydrate to the reaction solution of methyl p-aminosalicylate, use 10% sodium carbonate or 10% acetic acid to control the pH range of the reaction solution to be 6.5-7.5, and control the temperature at 35- 40°C, add 50.0g acetylase, strictly control the temperature and pH, react for 1 hour, and the reaction is complete. Methanol was recovered under reduced pressure, 500g of ethyl acetate was added to the mother liquor for extraction, liquid separation was carried out, drying and concentration was carried out, and then after cooling, crystallization and suction filtration, 195.9g of methyl para-acetamidosalicylate was obtained by air-drying at 50°C. Yield 93.6%...

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Abstract

The invention discloses a preparation method of ethopabate. Initially, para-aminosalicylic acid and p-toluene sulfonic acid are dissolved in methanol to form a mixed solution, the mixed solution is put in a reaction bottle, evenly stirred and heated, and a thermal insulation reaction is carried out; sodium acetate is added into a methyl p-aminosalicylate reaction liquid, the pH and temperature ofthe reaction liquid are controlled, acetylase is added, and a reaction is carried out to obtain methyl p-acetaminosalicylate; methyl p-acetaminosalicylate is added into acetone, heating is carried out, diethyl sulfate is added dropwisely, and after adding dropwisely is completed, a reaction is carried out to obtain ethopabate. The method has the advantages that industrial production can be achieved, resource conservation and environmental protection can be achieved, the cost can be better saved, the product quality is stable, the yield is high, and the method is suitable for large-scale industrial stable production.

Description

technical field [0001] The invention belongs to the technical field of chemical drug synthesis, and in particular relates to a preparation method of ethopabate. Background technique [0002] Ethoxyabate, the chemical name is 2-ethoxy-4-acetamidobenzoic acid methyl ester, also known as ethoba or coccidiodin, is a broad-spectrum anticoccidial veterinary drug and an important feed additive. [0003] Coccidiosis is a type of parasitic disease caused by single-celled protozoa entering the intestinal tract. The coccidia that infect chickens are mainly the Eimeria genus of Eimaceae, especially Eimeria tenabilis and poisonous Eimeria are the most harmful. If chickens are infected with coccidia oocysts, the oocysts will develop in the body and continue to reproduce sexually and asexually on the intestinal epithelial cells, secrete toxins, destroy the intestinal mucosal structure, and cause digestive dysfunction and bacterial infection. [0004] At present, coccidiosis has become th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/12C07C233/54
Inventor 蚩晓娜谷志勇吕亚军
Owner XUCHANG HENGSHENG PHARMA
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