Preparation method of carbasalate calcium

A technology of carbasalate calcium and aspirin, which is applied in the field of veterinary drug preparation, can solve problems such as poor product quality controllability, high production cost, and insufficient reaction, and achieve the effects of facilitating industrial production, reducing equipment requirements, and low production cost

Active Publication Date: 2013-02-13
QILU ANIMAL HEALTH PROD +1
View PDF5 Cites 18 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of carbasalate calcium
  • Preparation method of carbasalate calcium
  • Preparation method of carbasalate calcium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A preparation method of carbasalate calcium, the steps are as follows:

[0031] (1) Add 100g of aspirin, 46g of calcium nitrate and 20g of urea in sequence to 300ml of methanol, and stir at room temperature for 30min; then cool down, and add 35mL of ammonia water at a rate of 1-2ml per minute at 0-2°C while stirring, Then the temperature was raised to 32-35°C and reacted for 2 hours to obtain the reaction solution;

[0032] (2) Cool the reaction solution prepared in step (1) to 2-4°C, grow the crystal for 1 hour, then filter it with suction, and dry it in vacuum at 45-50°C for 3.5 hours to obtain 118 g of carbasalate calcium. The rate is 93%.

[0033] The test results of sample content and related substances are shown in Table 1, and the test results of sample stability are shown in Table 2.

Embodiment 2

[0035] A preparation method of carbasalate calcium, the steps are as follows:

[0036] (1) Add 100g of aspirin, 46g of calcium nitrate, and 20g of urea to 250mL of ethanol in sequence, stir and dissolve at room temperature for 30min; then cool down, and add 34mL of ammonia water at a rate of 1-2ml per minute at 2-4°C while stirring , and then heated up to 30-33°C, and reacted for 2 hours to obtain a reaction solution;

[0037] (2) Cool the reaction solution prepared in step (1) to 3-5°C, grow the crystal for 1 hour, then filter it with suction, and dry it in vacuum at 45-50°C for 4 hours to prepare 120 g of carbasalate calcium. The rate is 95%.

[0038] The obtained carbasalate calcium was confirmed by infrared spectrum, mass spectrum and nuclear magnetic resonance structure, and the results were as follows: Figure 1~3 shown.

[0039] The test results of sample content and related substances are shown in Table 1, and the test results of sample stability are shown in Table ...

Embodiment 3

[0041] A preparation method of carbasalate calcium, the steps are as follows:

[0042] (1) Add 100g of aspirin, 46g of calcium nitrate, and 20g of urea to 200mL of ethanol in sequence, stir and disperse at room temperature for 30min; then cool down, add 38mL of ammonia water at a rate of 1-2ml per minute under stirring at 3-5°C , and then heated up to 25-28°C, and reacted for 2 hours to obtain a reaction solution;

[0043] (2) Cool the reaction solution prepared in step (1) to 0-2°C, grow the crystal for 1 hour, then filter it with suction, and dry it in vacuum at 45-50°C for 3 hours to obtain 118 g of carbasalate calcium, which was harvested The rate is 93%.

[0044] The test results of sample content and related substances are shown in Table 1, and the test results of sample stability are shown in Table 2.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a preparation method of carbasalate calcium. The preparation method comprises the following steps: (1) dispersing aspirin, calcium nitrate and urea into alcohol, adding ammonia water under a stirring condition at 0-5 DEG C, then heating up to 25-35 DEG C, and reacting for 2-2.5 hours; and (2) cooling the reaction solution obtained in step (1) to 0-5 DEG C, standing for growing crystals, and then performing suction filtration and drying to obtain carbasalate calcium. The preparation method of arbasalate calcium is characterized by high product content, low content of impurities (related substances), good stability, concise process and low production cost; and the requirement on equipment is lowered, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of carbasalate calcium, belonging to the technical field of veterinary drug preparation. Background technique [0002] Carbasalate calcium is an antipyretic and analgesic drug. This product is a complex salt of calcium acetylsalicylate and urea, which 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. [0003] At present, the method for preparing carbasalate calcium mainly contains following three kinds: [0004] (i) Using acetone and ethanol as a mixed solvent, add aspirin, calcium nitrate tetrahydrate, and urea in sequence, and pass through ammonia g...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07C275/02C07C273/02C07C69/157C07C67/28
Inventor 刘全才孙兴林孔梅王希超吴连勇
Owner QILU ANIMAL HEALTH PROD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap