CN106496074B - A kind of preparation method of carbasalate calcium - Google Patents
A kind of preparation method of carbasalate calcium Download PDFInfo
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- CN106496074B CN106496074B CN201610791082.5A CN201610791082A CN106496074B CN 106496074 B CN106496074 B CN 106496074B CN 201610791082 A CN201610791082 A CN 201610791082A CN 106496074 B CN106496074 B CN 106496074B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/28—Preparation of carboxylic acid esters by modifying the hydroxylic moiety of the ester, such modification not being an introduction of an ester group
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of preparation method of carbasalate calcium, for making veterinary drug carbasalate calcium, includes the following steps；Urea is dissolved in the water, aspirin is added in into the solution, stirs, aspirin is made fully to dissolve, solution is added dropwise in the solution of calcium hydroxide water, stirs 10min, filtering；Filtrate is spray-dried, obtains carbasalate calcium.The present invention use water as solvent, cheap, also, due to not introducing organic solvent, will not generate poisonous and harmful substance, safety and environmental protection, yield height, suitable for mass producing.
Description
Technical field
The present invention relates to a kind of preparation methods of carbasalate calcium, the especially preparation method of veterinary drug carbasalate calcium, belong to
Field of pharmaceutical technology.
Background technology
Carbasalate calcium is aspirin (acetylsalicylic acid) derivative, is the complex compound of tylcalsin and urea, changes
Scientific name is double (2 one globentyl) ureas.The metabolic characteristic of carbasalate calcium and pharmacological action are identical with aspirin,
Acetylsalicylic acid is hydrolyzed in water and plays antipyretic, analgesia, anti-inflammatory and inhibition platelet aggregation.Carbasalate calcium can be used for
The fever of the various animals such as pig, chicken, ox and inflammation, it can also be used to which the kidney for alleviating chicken swells and remove uric acid mineralization, it may also be used for
The auxiliary treatment of febrile disease such as bird flu, ewcastle disease.
The content of the invention
The present invention is directed to the drawback of the prior art, provides a kind of preparation method of carbasalate calcium, is ensureing the same of yield
When using organic solvent, there is safety and environmental protection.
Technical problem of the present invention solves by the following technical programs；
A kind of preparation method of carbasalate calcium, preparation process are as follows：
A. urea is dissolved in the water, aspirin is added in into the solution, stirred, aspirin is made fully to dissolve, made
Urea-aspirin solution is obtained, urea-aspirin solution obtained is cooled to 0-5 DEG C；
B. calcium hydroxide is dispersed in water, keeps 0-5 DEG C of temperature, be added dropwise what a steps obtained into calcium hydroxide solution
Urea-aspirin solution is made；
C. after being added dropwise, 0-5 DEG C of temperature is kept, stirs 10min, filtering takes filtrate；
D. 0-5 DEG C of temperature is kept, the filtrate that spray drying step c obtains, the filter residue that step c obtains is as next batch reaction
Raw material is continuing with.
The preparation method of above-mentioned carbasalate calcium, the temperature control of each step are as follows：
A. urea is dissolved in the water, aspirin is added in into the solution, stirred, aspirin is made fully to dissolve, made
Urea-aspirin solution is obtained, urea-aspirin solution obtained is cooled to 0 DEG C；
B. calcium hydroxide is dispersed in water, keeps 0 DEG C of temperature, the system that a steps obtain is added dropwise into calcium hydroxide solution
Obtain urea-aspirin solution；
C. after being added dropwise, 0 DEG C of temperature is kept, stirs 10min, filtering takes filtrate；
D. 0 DEG C of temperature is kept, the filtrate that spray drying step c obtains, the filter residue that step c obtains is as next batch reaction original
Material is continuing with.
The preparation method of above-mentioned carbasalate calcium, each component are calculated by weight as：1-4 parts of urea, aspirin 18-21
Part, 2-4 parts of calcium hydroxide, 40-60 parts of the water of dissolved urea dissolves 20-40 parts of the water of calcium hydroxide.
The present invention has the following advantages：
The present invention uses water as solvent, cheap, also, due to not introducing organic solvent, and will not generate toxic has
Evil substance, safety and environmental protection；Contain aspirin in filter residue after filtering, can use, avoid as next group reaction raw materials
Waste；Technique is easy to operation, reduces labor intensity, is suitble to industrialized production；The method of the invention, high income can reach
95% or so.
Specific embodiment
Embodiment 1
A. remember by weight, urea be dissolved in 50 parts of water for 2 parts, 18 parts of aspirin is added in into the solution, stir,
Aspirin is made fully to dissolve, 6 parts of solution is made as stated above, solution is cooled to 0 DEG C respectively, 1 DEG C, 2 DEG C, 3 DEG C, 4 DEG C, and 5
℃；
B. by calcium hydroxide 2 parts be scattered in 40 parts of water, keep a steps temperature, into the solution be added dropwise a steps obtain
Solution；
C. after being added dropwise, the temperature of a steps is kept, stirs 10min, filtering；
D. the temperature of a steps is kept, is spray-dried the solution that step c obtains, the filter residue that step c obtains is anti-as next group
Raw material is answered to be continuing with.The yield measured at each temperature enters such as the following table 1.
The material yield measured at a temperature of 1 differential responses of table
| Temperature (DEG C) | 0 | 1 | 2 | 3 | 4 | 5 |
| Yield (%) | 96 | 95.6 | 95.1 | 94.8 | 94.5 | 94 |
Embodiment 2
A. remember by weight, urea be dissolved in 40 parts of water for 1 part, 18 parts of aspirin is added in into the solution, stir,
Aspirin is made fully to dissolve, solution is cooled to 0 DEG C；
B. by calcium hydroxide 2 parts be scattered in 20 parts of water, keep 0 DEG C of temperature, into the solution be added dropwise a steps obtain it is molten
Liquid；
C. after being added dropwise, 0 DEG C of temperature is kept, stirs 10min, filtering；
D. 0 DEG C of temperature is kept, the solution that spray drying step c obtains, the filter residue that step c obtains is as next batch reaction original
Material is continuing with.Measured yield 94%.
Embodiment 3
A. remember by weight, urea be dissolved in 60 parts of water for 4 parts, 21 parts of aspirin is added in into the solution, stir,
Aspirin is made fully to dissolve, solution is cooled to 0 DEG C；
B. by calcium hydroxide 4 parts be scattered in 40 parts of water, keep 0 DEG C of temperature, into the solution be added dropwise a steps obtain it is molten
Liquid；
C. after being added dropwise, 0 DEG C of temperature is kept, stirs 10min, filtering；
D. 0 DEG C of temperature is kept, the solution that spray drying step c obtains, the filter residue that step c obtains is as next batch reaction original
Material is continuing with.Measured yield 93%.
Embodiment 4
A. remember by weight, urea be dissolved in 50 parts of water for 3 parts, 19 parts of aspirin is added in into the solution, stir,
Aspirin is made fully to dissolve, solution is cooled to 0 DEG C；
B. by calcium hydroxide 3.7 parts be scattered in 30 parts of water, keep 0 DEG C of temperature, a steps be added dropwise into the solution and obtain
Solution；
C. after being added dropwise, 0 DEG C of temperature is kept, stirs 10min, filtering；
D. 0 DEG C of temperature is kept, the solution that spray drying step c obtains, the filter residue that step c obtains is as next batch reaction original
Material is continuing with.Measured yield 98%.
Embodiment 5
A. remember by weight, urea be dissolved in 55 parts of water for 2 parts, 20 parts of aspirin is added in into the solution, stir,
Aspirin is made fully to dissolve, solution is cooled to 0 DEG C；
B. by calcium hydroxide 3 parts be scattered in 35 parts of water, keep 0 DEG C of temperature, into the solution be added dropwise a steps obtain it is molten
Liquid；
C. after being added dropwise, 0 DEG C of temperature is kept, stirs 10min, filtering；
D. 0 DEG C of temperature is kept, the solution that spray drying step c obtains, the filter residue that step c obtains is as next batch reaction original
Material is continuing with.Measured yield 95%.
Embodiment 6
A. remember by weight, urea be dissolved in 45 parts of water for 2.5 parts, 18.5 parts of aspirin is added in into the solution,
Stirring, makes aspirin fully dissolve, solution is cooled to 0 DEG C；
B. by calcium hydroxide 1.5 parts be scattered in 35 parts of water, keep 0 DEG C of temperature, a steps be added dropwise into the solution and obtain
Solution；
C. after being added dropwise, 0 DEG C of temperature is kept, stirs 10min, filtering；
D. 0 DEG C of temperature is kept, the solution that spray drying step c obtains, the filter residue that step c obtains is as next batch reaction original
Material is continuing with.Measured yield 96%.
Claims (3)
1. a kind of preparation method of carbasalate calcium, which is characterized in that preparation process is as follows：
A. urea is dissolved in the water, aspirin is added in into the solution, stirred, aspirin is made fully to dissolve, urine is made
Urea-aspirin solution obtained is cooled to 0-5 DEG C by element-aspirin solution；
B. calcium hydroxide is dispersed in water, keeps 0-5 DEG C of temperature, what dropwise addition a steps obtained into calcium hydroxide solution is made
Urea-aspirin solution；
C. after being added dropwise, 0-5 DEG C of temperature is kept, stirs 10min, filtering takes filtrate；
D. 0-5 DEG C of temperature is kept, the filtrate that spray drying step c obtains, the filter residue that step c obtains is as next group reaction raw materials
It is continuing with.
2. a kind of preparation method of carbasalate calcium, which is characterized in that the temperature control of each step is as follows：
A. urea is dissolved in the water, aspirin is added in into the solution, stirred, aspirin is made fully to dissolve, urine is made
Urea-aspirin solution obtained is cooled to 0 DEG C by element-aspirin solution；
B. calcium hydroxide is dispersed in water, keeps 0 DEG C of temperature, the obtained urine that a steps obtain is added dropwise into calcium hydroxide solution
Element-aspirin solution；
C. after being added dropwise, 0 DEG C of temperature is kept, stirs 10min, filtering takes filtrate；
D. keep 0 DEG C of temperature, the obtained filtrate of spray drying step c, the filter residue that step c obtains as next group reaction raw materials after
It is continuous to use.
3. the preparation method of a kind of carbasalate calcium according to claim 1, which is characterized in that each component is in parts by weight
It is calculated as：1-4 parts of urea, 18-21 parts of aspirin, 2-4 parts of calcium hydroxide, 40-60 parts of the water of dissolved urea dissolve calcium hydroxide
20-40 parts of water.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107344919A (en) * | 2017-05-27 | 2017-11-14 | 山东久隆恒信药业有限公司 | A kind of preparation method of carbasalate calcium |
| CN109134315A (en) * | 2017-06-19 | 2019-01-04 | 河南后羿制药有限公司 | A kind of preparation method of carbasalate calcium and carbasalate calcium prepared by this method |
| CN107619383B (en) * | 2017-07-21 | 2020-10-27 | 河北师范大学 | Method for preparing carbasalate calcium microcrystal powder |
| CN109111378A (en) * | 2018-10-29 | 2019-01-01 | 河南后羿实业集团有限公司 | A kind of preparation method of carbasalate calcium |
| CN110724057B (en) * | 2019-12-05 | 2023-03-31 | 山东省化工研究院 | Preparation method of carbasalate calcium |
| CN112321459A (en) * | 2020-11-25 | 2021-02-05 | 济南久隆医药科技有限公司 | Method for synthesizing carbasalate calcium |
| CN114315574A (en) * | 2021-12-31 | 2022-04-12 | 河南豫辰药业股份有限公司 | Preparation method of carbasalate calcium |
| CN115572227A (en) * | 2022-10-14 | 2023-01-06 | 枣庄市润安制药新材料有限公司 | Method for preparing carbasalate calcium |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102382013A (en) * | 2011-08-16 | 2012-03-21 | 青岛康地恩药业股份有限公司 | Preparation method of carbasalate calcium |
| CN102924335A (en) * | 2012-11-13 | 2013-02-13 | 齐鲁动物保健品有限公司 | Preparation method of carbasalate calcium |
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- 2016-08-31 CN CN201610791082.5A patent/CN106496074B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102382013A (en) * | 2011-08-16 | 2012-03-21 | 青岛康地恩药业股份有限公司 | Preparation method of carbasalate calcium |
| CN102924335A (en) * | 2012-11-13 | 2013-02-13 | 齐鲁动物保健品有限公司 | Preparation method of carbasalate calcium |
Non-Patent Citations (1)
| Title |
|---|
| 卡巴匹林钙的一锅烩合成工艺改进;梁久来 等;《中国药物化学杂志》;20010630;第11卷(第3期);实验部分 * |
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