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Preparation method of carbasalate calcium

A technology of carbasalate calcium and aspirin, which is applied in the field of veterinary drug preparation, can solve the problems of high production cost, low product content, excessive ammonia gas, etc., and achieves the effects of reducing equipment requirements, low equipment requirements and high safety.

Inactive Publication Date: 2017-11-14
SHANDONG JIULONG HISINCE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are problems in this process: acetone and ethanol are used as a mixed solvent, which is difficult to separate and recover, which causes certain difficulties in production; the end point of the ammonia gas reaction is not easy to control in production, and the production risk factor is high.
The method has the following problems: the use of ammonia in industrial production is cumbersome, and the reaction end point of the method is not easy to control: insufficient ammonia, insufficient reaction, excessive ammonia, product content decline, high impurity salicylic acid, product Poor quality controllability
This method has the following problems: ethylene glycol monomethyl ether is a highly toxic solvent, and long-term contact can cause irreversible damage to the hematopoietic system; ethylene glycol monomethyl ether has a high boiling point and is difficult to recycle, resulting in high production costs; Ether is easy to adsorb on the product, and the residue is not easy to remove. It needs to be cleaned with ether, so there is a safety hazard; the yield is 74%, the yield is low, the product content is low, and the impurities are high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 50g of aspirin and 25g of urea to 400g of ethanol, raise the temperature to 42°C and dissolve them all. As liquid A, dissolve 25g of calcium propionate in 75g of purified water at 25°C. As liquid B, add liquid B to liquid A dropwise at 45°C During the process, the dropping rate was controlled, and the dripping was completed at a constant speed for 30 minutes. The reaction was stirred for 5 hours, and the temperature was lowered to 5°C. At this time, a large amount of crystals were precipitated, centrifuged, and dried to obtain carbasalate calcium, with a yield of 98.1% and a purity of 99.2%.

Embodiment 2

[0022] Add 50g of aspirin and 25g of urea into 50g of ethanol, raise the temperature to 40°C and dissolve them all, as liquid A, dissolve 25g of calcium propionate in 60g of purified water at 20°C, as liquid B, add liquid B to liquid A dropwise at 40°C During the process, the dropping rate was controlled, and the dripping was completed at a constant speed for 30 minutes. The reaction was stirred for 5 hours, and the temperature was lowered to 0°C. At this time, a large amount of crystals were precipitated, centrifuged, and dried to obtain carbasalate calcium. The yield was 97.1%, and the purity was 99.3%.

Embodiment 3

[0024] Add 50g of aspirin and 25g of urea to 500g of ethanol, heat up to 50°C and dissolve them all. As liquid A, dissolve 25g of calcium propionate in 90g of purified water at 30°C. As liquid B, add liquid B to liquid A dropwise at 50°C During the process, the dropping rate was controlled, and the dripping was completed at a constant speed for 30 minutes. The reaction was stirred for 5 hours, and the temperature was lowered to 10°C. At this time, a large amount of crystals were precipitated, centrifuged, and dried to obtain carbapirin calcium. The yield was 97.8%, and the purity was 99.1%.

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PUM

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Abstract

The invention relates to a preparation method of carbasalate calcium. The preparation method comprises the following steps of adding aspirin and urea in alcohol, rising the temperature to enable the aspirin and the urea to be dissolved as liquid A, dissolving a calcium source into purified water as liquid B, dropwise adding the liquid B in the liquid A at high temperature, carrying out reaction for 5h, cooling for crystallization, wherein a great amount of crystals are separated out at the time, and carrying out centrifugation and drying to obtain the carbasalate calcium. The carbasalate calcium prepared by the preparation method of the technology is high in content, little in impurity and good in stability; and in addition, the technology is simple, is liable to operate, lowers the requirements for equipment and is beneficial to industrial mass production.

Description

technical field [0001] The invention belongs to the technical field of veterinary drug preparation, and relates to a preparation method for drug synthesis, in particular to a preparation method for antipyretic and analgesic drug carbapirin calcium. Background technique [0002] Carbasalate calcium is an antipyretic and analgesic drug, which is a derivative of aspirin (acetylsalicylic acid). It is hydrolyzed into acetylsalicylic acid in the body to exert antipyretic, analgesic and anti-inflammatory effects. It can be used for fever and inflammation of various animals such as pigs, chickens, and cattle. It can also be used to relieve kidney swelling and remove urate deposits in chickens. It can also be used as an adjuvant treatment for febrile diseases such as avian influenza and Newcastle disease. Compared with aspirin, carbasalate calcium has fewer side effects and better water solubility, so it has received widespread attention. [0003] At present, the method for prepari...

Claims

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Application Information

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IPC IPC(8): C07C273/02C07C275/02C07C67/28C07C69/157
CPCC07C273/02C07C67/28C07C275/02C07C69/157
Inventor 殷习栋李志远杨统鹏韩伟胡文婷刘丕雷宋晶晶
Owner SHANDONG JIULONG HISINCE PHARMA CO LTD
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