Synthesis process of carbaspirin calcium

A technology of carbasalate calcium and synthesis process is applied in the synthesis process of carbasalate calcium and in the field of preparation of organic medicines, which can solve the problems of high price and high production cost, reduce the cost of raw materials, ensure quality, and simplify the production process. Effect

Active Publication Date: 2020-02-11
山东青科农牧发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing production processes all use aspirin as the starting material, which is expensive and has high production costs

Method used

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  • Synthesis process of carbaspirin calcium
  • Synthesis process of carbaspirin calcium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add ethanol 180g, salicylic acid 276.24g (2mol), acetic anhydride 204.18g (2mol) successively in the 2L there-necked flask with reflux condenser and stirring, start stirring, add calcium carbonate 100.09g (1mol) in batches ( Divide the calcium carbonate into portions, add once every 10 minutes, and the amount added each time is 1.5 times the amount added before, and the addition is completed within 2 hours. The added amounts are 0.26g, 0.39g, 0.58g, 0.87g, 1.3 g..., until the addition is complete), the temperature is raised to 60°C, kept for 0.5h, and then cooled to 25°C. Then add 122.16g (2mol) of ethanolamine, 330.33g of pure water, and 66.07g of urea (1.1mol, the mass ratio of water to urea is 10:2), and the reaction time is 1h. After the reaction, cool down to 15°C, centrifuge, and rinse with 50g of ethanol , drying to obtain high-quality carbasalate calcium.

Embodiment 2

[0033] Add 180g of ethanol, 276.24g of salicylic acid, and 204.18g of acetic anhydride in sequence in a 2L three-necked flask with reflux condenser and stirring, start stirring, and add 100.09g of calcium carbonate in batches (calcium carbonate is divided into portions, every 15min Add once, and the amount added each time is 1.5 times the amount added before, and the addition is completed within 2.5 hours), the temperature is raised to 65°C, kept for 1h, and the temperature is lowered to 30°C. Then add 122.16g of ethanolamine, 330.33g of pure water, and 66.07g of urea (the mass ratio of water to urea is 10:2), and the reaction time is 2h. After the reaction, the temperature is lowered to 20°C, centrifuged, rinsed with 50g of ethanol, and dried to obtain high-quality carbasalate calcium.

Embodiment 3

[0035] Add 180g of ethanol, 276.24g of salicylic acid, and 204.18g of acetic anhydride in sequence in a 2L three-neck flask with reflux condenser and stirring, start stirring, and add 100.09g of calcium carbonate in batches (calcium carbonate is divided into portions, every 20min Add once, and the amount added each time is 1.5 times the amount added before, and the addition is completed within 3 hours), the temperature is raised to 60°C, kept for 0.5h, and the temperature is lowered to 30°C. Then add 122.16 g of ethanolamine, 360 g of pure water, and 66.07 g of urea. The reaction time is 3 hours. After the reaction, the temperature is lowered to 15° C., centrifuged, rinsed with 50 g of ethanol, and dried to obtain high-quality carbasalate calcium.

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Abstract

The invention discloses a synthesis process of carbaspirin calcium. The synthesis process comprises the following production procedures: adding a certain amount of ethanol, salicylic acid and acetic anhydride into a three-neck flask, starting stirring, adding calcium carbonate in batches, carrying out heating to a certain temperature, performing a reaction for a period of time, carrying out cooling to a certain temperature, adding a certain amount of water, ethanolamine and urea, maintaining the temperature for 2 h, and after the reaction is finished, successively carrying out cooling, centrifuging, leaching and drying to obtain the high-quality carbaspirin calcium.

Description

technical field [0001] The invention relates to a preparation method of an organic drug, in particular to a synthesis process of carbapirin calcium, which belongs to the field of chemical synthesis. Background technique [0002] Carbasalate Calcium (Carbasalate Calcium) is an aspirin derivative, and its chemical name is bis-(2-acetoxybenzoic acid) urea. Because the product has high bioavailability, small side effects and good water solubility, its curative effect is similar to that of aspirin. Widely valued, it is currently the only antipyretic and analgesic drug approved by relevant departments in my country for oral administration of livestock and poultry, and belongs to the third category of new veterinary drugs in the country. The European Union has approved carbasalate calcium to be used in all food animals except aquatic animals, and the U.S. FDA has also listed it as an over-the-counter drug. It has been used clinically in foreign countries, and it has also been approv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/28C07C69/157C07C273/02C07C275/02
CPCC07C67/28C07C273/02C07C69/157C07C275/02
Inventor 岳涛李培培刘启奎杨松梁辉张晓霞
Owner 山东青科农牧发展有限公司
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