A kind of synthetic technique of carbasalate calcium

A technology of carbasalate calcium and synthesis process is applied in the synthesis process of carbasalate calcium and the preparation field of organic medicines, and can solve the problems of high production cost, high price and the like, and achieves reduction in raw material cost, improvement in yield, and simplification of production. The effect of the process flow

Active Publication Date: 2022-04-26
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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  • A kind of synthetic technique of carbasalate calcium
  • A kind of synthetic technique of carbasalate calcium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031]In a 2L three-mouth flask with reflux condensing tube and stirring, 180g ethanol, 276.24g (2mol) of salicylic acid, 204.18g (2mol) of acetic anhydride were added sequentially, stirred, and 100.09g (1mol) of calcium carbonate was added in batches (the calcium carbonate was divided, added once every 10min, and each addition amount was 1.5 times the previous addition amount, added within 2 hours, the addition amount was 0.26g, 0.39g, 0.58g, 0.87g, 1.3 g ..., until the addition is completed), heat up to 60 °C, keep warm for 0.5 h, cool down to 25 °C. Then add ethanolamine 122.16g (2mol), pure water 330.33g, urea 66.07g (1.1mol, water to urea mass ratio of 10:2), reaction time 1h, after the end of the reaction cooled to 15 °C, centrifugation, 50g ethanol leaching, drying, to obtain high-quality carbapiplin calcium.

Embodiment 2

[0033] In a 2L three-mouth flask with reflux condensing tube and stirring, 180g of ethanol, 276.24g of salicylic acid, and 204.18g of acetic anhydride were added sequentially, stirred, and 100.09g of calcium carbonate was added in batches (the calcium carbonate was divided into parts, added every 15min, and each addition amount was 1.5 times the amount of the previous addition, added within 2.5h), heated to 65 °C, kept warm for 1h, and cooled to 30 °C. Then add ethanolamine 122.16g, pure water 330.33g, urea 66.07g (water and urea mass ratio of 10:2), reaction time 2h, after the end of the reaction cooled to 20 °C, centrifugation, 50g ethanol leaching, drying, to obtain high-quality carbapipillin calcium.

Embodiment 3

[0035] In a 2L three-mouth flask with reflux condensing tube and stirring, 180g of ethanol, 276.24g of salicylic acid, and 204.18g of acetic anhydride were added sequentially, stirred, and 100.09g of calcium carbonate was added in batches (the calcium carbonate was divided into parts, added every 20min, and each addition amount was 1.5 times the previous addition amount, added within 3h), heated to 60 °C, insulation 0.5h, cooled to 30 °C. Then add ethanolamine 122.16g, pure water 360g, urea 66.07g, reaction time 3h, after the end of the reaction cooled to 15 °C, centrifugation, 50g ethanol leaching, drying, to obtain high-quality carbapiprin calcium.

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Abstract

The invention discloses a synthesis process of carbasalate calcium. The production process is as follows: add a certain amount of ethanol, salicylic acid, and acetic anhydride into a three-necked flask, start stirring, add calcium carbonate in batches, and heat up to a certain level. After a period of reaction, the temperature is lowered to a certain temperature, and then a certain amount of water, ethanolamine and urea are added, and the temperature is kept for 2 hours. After the reaction is completed, the temperature is lowered, centrifuged, rinsed, and dried to obtain high-quality carbasalate calcium.

Description

Technical field [0001] The present invention relates to a method for preparing an organic drug, specifically, to a synthesis process of carbapiplin calcium, belonging to the field of chemical synthesis. Background [0002] Carbasalate Calcium (Carbasalate Calcium) is an aspirin derivative, chemical name bis-(2-acetoxybenzoic acid)urea, due to the high bioavailability of the product, small side effects and good water solubility, the efficacy is similar to aspirin, so it has been widely valued, is currently the only approved by the relevant departments in China for livestock and poultry oral antipyretic analgesic drugs, belongs to the national three types of new veterinary drugs. The European Union has approved kabapirin calcium for all food animals except aquatic animals, and the US FDA has also listed it as an over-the-counter drug, which has been applied to the clinic abroad and approved in human medicine at home. [0003] At present, from the published patent point of view of ...

Claims

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Application Information

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Patent Type & Authority Patents(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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