Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of bis(2-acetoxybenzoic acid) calcium urea compound

A technology of acetoxybenzoic acid and compounds, which is applied in the field of preparation of dicalcium urea compounds, can solve problems such as poor quality of final products, unclarified reaction liquid, hidden dangers of safety, etc., and achieve stable product quality, easy control of reaction conditions, The effect of low production cost

Active Publication Date: 2021-04-02
SHANDONG XINHUA PHARMA CO LTD
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method is relatively simple to operate, there are many problems in the preparation process. The calcium nitrate used in the method is anhydrous calcium nitrate, which is explosive and has potential safety hazards.
The reaction material is dispersed in alcohol, and the foreign matter in the material is not filtered out through the process of dissolution. At the same time, the reaction liquid is not clarified during the reaction process of adding ammonia water, which inevitably causes the reaction material to be trapped, resulting in incomplete reaction and final product quality. Poor, low yield

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 bis(2-acetoxybenzoic acid) calcium urea compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 360kg of anhydrous (recovery) ethanol in a 1000L reactor, add 15.6kg of urea and 36.1kg of calcium nitrate under stirring, heat up to 40°C, stir and dissolve for 15 minutes, then add 72kg of acetylsalicylic acid compound (Ⅲ) and continue stirring Dissolve for 15 minutes, press filter, wash with 40kg of anhydrous (recovered) ethanol, cool the filtrate to 0±3°C while stirring, control the rate of ammonia flow, and pass about 6.8-6.9kg of ammonia within 60 minutes (based on the pH of the reaction solution ≤7.4), the reaction produces calcium acetylsalicylate compound (II) under this condition and continued to stir for 10 minutes, and the re-measured pH value was between 7 and 7.4. Then the temperature is raised gradually, and the reaction temperature is raised from 0±3°C to 15°C, and the heating time is 20 minutes. At this time, the pH of the reaction solution is ≤7; <7, keep warm for complexation reaction for 1 hour; then raise the temperature to 37±2°C, keep warm for...

Embodiment 2

[0028] Add 504kg of anhydrous (recovery) ethanol in a 1000L reactor, add 16.8kg of urea and 35.3kg of calcium nitrate under stirring, heat up to 50°C, stir and dissolve for 10 minutes, then add 72kg of acetylsalicylic acid compound (Ⅲ) and continue stirring Dissolve for 10 minutes, press filter, wash with 20kg of anhydrous (recovered) ethanol, cool the filtrate to 0±3°C under stirring, control the speed of ammonia flow, and pass in about 6.8-6.9kg of ammonia in 30 minutes (based on the pH of the reaction solution≤ 7.4 as the standard), the reaction generates calcium acetylsalicylate compound (II) under this condition and continued to stir for 10 minutes, and the re-measured pH value was between 7 and 7.4. Then the temperature is raised gradually, and the reaction temperature is raised from 0±3°C to 10°C for 30 minutes. At this time, the pH of the reaction solution is ≤7; <7, keep warm for complexation reaction for 1 hour; then raise the temperature to 37±2°C, keep warm for 1 h...

Embodiment 3

[0031] Add 432kg of anhydrous (recovery) ethanol in a 1000L reactor, add 14.4kg of urea and 34.4kg of calcium nitrate under stirring, heat up to 45°C, stir and dissolve for 13 minutes, then add 72kg of acetylsalicylic acid compound (Ⅲ) and continue stirring Dissolve for 13 minutes, press filter, wash with 30kg of anhydrous (recovered) ethanol, cool the filtrate to 0±3°C while stirring, control the rate of ammonia flow, and pass about 6.8-6.9kg of ammonia in 45 minutes (based on the pH of the reaction solution≤ 7.4 as the standard), the reaction generates calcium acetylsalicylate compound (II) under this condition and continued to stir for 10 minutes, and the re-measured pH value was between 7 and 7.4. Then the temperature is raised gradually, and the reaction temperature is raised from 0±3°C to 13°C for 25 minutes. At this time, the pH of the reaction solution is ≤7; then the temperature is raised from 13°C to 30±3°C for 25 minutes. <7, keep warm for complexation reaction for ...

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 belongs to the technical field of medicine synthesis, and particularly relates to a preparation method of a bis(2-acetoxybenzoic acid)calcium-urea compound. The preparation method comprises the following steps: adding urea and calcium nitrate into solvent ethanol, heating, stirring, dissolving, adding an acetylsalicylic acid compound, continuously stirring, dissolving, press filtering, and cleaning; and cooling filtrate under a stirring effect, introducing ammonia gas, performing the calcification reaction to generate the calcium acetylsalicylate compound, then gradient increasing the temperature, performing the complexing reaction, generating the bis(2-acetoxybenzoic acid)calcium-urea compound, and performing the after-treatment. The process is stable, the reaction conditionis mild and easy to control, the preparation and purification process is simple in operation, the yield is high, the product quality is stable, the HPLC content is 99.8 percent or more, and the content of single major impurity salicylic acid is less than 0.1 percent; and the after-treatment is simple, the recycled solvent can be continuously used, less waste gas, waste water and waste solid are produced, the production cost is low, and the industrialized production can be realized.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a preparation method of bis(2-acetoxybenzoic acid) calcium urea compound. Background technique [0002] Bis(2-acetoxybenzoic acid) calcium urea is a derivative of acetylsalicylic acid. This product is a complex salt of calcium acetylsalicylate and urea. It is hydrolyzed into acetylsalicylic acid in water to exert antipyretic, analgesic and anti-inflammatory effects. Its curative effect is the same as that of aspirin, with low side effects and good water solubility. For headache, toothache, fever and pain during cold and cold, fever and pain after vaccination, neuralgia, low back pain, muscle pain and menstrual pain. It is the only antipyretic and analgesic drug approved in the world for all food animals such as pigs, chickens, cattle, and rabbits, and has been included in the European Pharmacopoeia. It is a national third-class new veterinary drug, and th...

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 Patents(China)
IPC IPC(8): C07C67/00C07C69/157C07C273/02C07C275/02
CPCC07C67/00C07C67/28C07C273/02C07C69/157C07C275/02
Inventor 朱连博
Owner SHANDONG XINHUA PHARMA CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com