CN105294481B - A kind of preparation method of quadracycline - Google Patents
A kind of preparation method of quadracycline Download PDFInfo
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- CN105294481B CN105294481B CN201510801097.0A CN201510801097A CN105294481B CN 105294481 B CN105294481 B CN 105294481B CN 201510801097 A CN201510801097 A CN 201510801097A CN 105294481 B CN105294481 B CN 105294481B
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- quadracycline
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Abstract
The present invention relates to a kind of preparation method of quadracycline, tetracycline and butanol are well mixed by this method first, adjust pH to 1.7~1.9, then 60~90 minutes are incubated after being to slowly warm up to 50~52 DEG C, decrease temperature crystalline, terminate rear vacuum drawn crystal solution, washed with acetone, drain, drying can obtain quadracycline.The present invention is using the step of tetracycline one generation quadracycline, because without urea double salt post, reduce one of post yield loss, simultaneously as a procedure is lacked, personnel are reduced, production equipment is reduced, urea material consumption is not present, reduce the production cost of product, the advantage that the technological process of production shortens, which is also embodied in, can timely handle intermediate material, storage, the processing time of intermediate material are greatly shortened, effectively reduces the probability that degradation reaction occurs for tetracycline, product quality is improved.
Description
Technical field
The present invention relates to biology and new medical technology, more particularly to a kind of preparation method of quadracycline.
Background technology
In the prior art, the production method of quadracycline is：Tetracycline and urea reaction are generated into urea double salt first,
Then urea double salt is dissolved in butanol, crystallization generation quadracycline.This method is converted into urea tetracycline in tetracycline
During, there are yield losses, the consumption of urea, personnel's wage, cause the production cost of product to raise.
The content of the invention
The defects of it is an object of the invention to overcome above-mentioned prior art, there is provided one kind effectively improves product yield, reduces
Labor intensity, production equipment and personnel are reduced, improve the preparation method of the quadracycline of the CLA of work production environment.
The technical scheme taken for achieving the above object is：
A kind of preparation method of quadracycline, it is characterised in that its step is：Tetracycline and butanol are mixed first equal
It is even, pH to 1.7~1.9 is adjusted, is incubated 60~90 minutes after being then to slowly warm up to 50~52 DEG C, decrease temperature crystalline, crystallization terminates
Vacuum drawn crystal solution afterwards, washed, drained with acetone, drying can obtain quadracycline.
The rate of charge of the tetracycline and butanol is 1：5~6.
The temperature control when butanol feeds intake is at 17~19 DEG C.
The pH adjustment concentrated sulfuric acid.
During the heating, temperature is risen to 50~52 DEG C with the time of 20-80 minutes.
The decrease temperature crystalline refers to feed temperature is down into 22~30 DEG C with 60~120 minutes, crystallized.
The present invention, because without urea double salt post, reduces one of hilllock using the step of tetracycline one generation quadracycline
Position yield loss, simultaneously as having lacked a procedure, personnel are reduced, and production equipment is reduced, and urea material consumption is not present, and reduces production
The production cost of product, the advantage that the technological process of production shortens, which is also embodied in, can timely handle intermediate material, greatly contract
The short storage of intermediate material, processing time, the probability that degradation reaction occurs for tetracycline is effectively reduced, product quality obtains
To raising.
Embodiment
The present invention is described in further detail by following examples, but the technology contents that are described of the present embodiment be it is illustrative,
Rather than it is limited, protection scope of the present invention should not be limited to according to this, within the spirit and principles of the invention, made
Any modification, equivalent substitution and improvements etc., should be included in the scope of the protection.
The reductive hydrolysis reaction solution of CLA in following embodiments is erythromycin thiocyanate oximation reaction, is etherified instead
Should, it obtain after Silanization reaction, methylation reaction and reductive hydrolysis reaction.
Embodiment 1
Weigh 100g, the wet alkali of tetracycline of moisture content 15%.(given money as a gift) according to tetracycline：Butanol=1：5~6 rate of charges, amount
425ml butanol is taken, temperature is 17 DEG C.It is mixed evenly, is adjusted with 30ml concentrated hydrochloric acid, pH test paper determines solution in pH=
In the range of 1.7~1.9, solution clarification, it is 154501u/ml to determine its potency unit.Start to warm up, with 30 minutes by solution
Temperature rises to 51 DEG C, continues insulation 60 minutes, then temperature cools at 50~52 DEG C, temperature is down to 25 DEG C, and the used time 60 divides
Clock.Crystallization terminates.Vacuum drawn crystal solution, washed, drained with 120ml acetone, the quadracycline after extraction is wet
Product, it is put into baking oven and is dried, taken out after 30 minutes, claim to obtain quadracycline 67g, determines its moisture content 0.33%.
Embodiment 2
Weigh 200g, the wet alkali of tetracycline of moisture content 15%.(given money as a gift) according to tetracycline：Butanol=1:5~6 rate of charges, amount
850ml butanol is taken, temperature is 17.5 DEG C.It is mixed evenly, is adjusted with 58ml concentrated hydrochloric acid, pH test paper determines solution in pH
In the range of=1.7~1.9, solution clarification, it is 162546u/ml to determine its potency unit.Start to warm up, will be molten with 35 minutes
Liquid temperature degree rises to 50 DEG C, continues insulation 60 minutes, then temperature cools at 50~52 ° DEG C, temperature is down to 25 DEG C, the used time
60 minutes.Crystallization terminates.Vacuum drawn crystal solution, washed, drained with 240ml acetone, by the hydrochloric acid Fourth Ring after extraction
Plain wet product, is put into baking oven and is dried, and is taken out after 30 minutes, claims to obtain quadracycline 131g, determines its moisture content 0.24%.
Embodiment 3
Weigh 1000g, the wet alkali of tetracycline of moisture content 15%.(given money as a gift) according to tetracycline：Butanol=1:5~6 rate of charges, amount
4250ml butanol is taken, temperature is 19 DEG C.It is mixed evenly, is adjusted with 290ml concentrated hydrochloric acid, pH test paper determines solution in pH
In the range of=1.7~1.9, solution clarification, it is 1491051u/ml to determine its potency unit.Start to warm up, will be molten with 30 minutes
Liquid temperature degree rises to 51 DEG C, continues insulation 60 minutes, then temperature cools at 50~52 DEG C, temperature is down to 25 DEG C, the used time 60
Minute.Crystallization terminates.Vacuum drawn crystal solution, washed, drained with 1200ml acetone, by the quadracycline after extraction
Wet product, it is put into baking oven and is dried, taken out after 30 minutes, claim to obtain quadracycline 663g, determines its moisture content 0.41%.
Claims (1)
1. a kind of preparation method of quadracycline, it is characterised in that its step is：First by tetracycline and butanol according to 1：5~
6 rate of charge is well mixed, and 17~19 DEG C of temperature when control butanol feeds intake, is added concentrated hydrochloric acid, is adjusted pH to 1.7~1.9, so
Temperature is risen to 50~52 DEG C with the time of 20-80 minutes afterwards, is incubated 60~90 minutes afterwards, with 60~120 minutes by feed liquid
Temperature is down to 22~30 DEG C of progress decrease temperature crystallines, terminates rear vacuum drawn crystal solution, is washed, drained with acetone, drying is
It can obtain quadracycline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510801097.0A CN105294481B (en) | 2015-11-19 | 2015-11-19 | A kind of preparation method of quadracycline |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510801097.0A CN105294481B (en) | 2015-11-19 | 2015-11-19 | A kind of preparation method of quadracycline |
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| CN105294481A CN105294481A (en) | 2016-02-03 |
| CN105294481B true CN105294481B (en) | 2017-12-22 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106086145A (en) * | 2016-06-14 | 2016-11-09 | 成都中牧生物药业有限公司 | A kind of synthesis technique of quadracycline |
| CN107954892A (en) * | 2017-12-22 | 2018-04-24 | 宁夏启元药业有限公司 | A kind of method of solvent residual amount in reduction quadracycline |
| CN111100900A (en) * | 2019-12-19 | 2020-05-05 | 河北圣雪大成制药有限责任公司 | Method for preparing demethyltetracycline by fermentation method |
| CN112521307A (en) * | 2020-12-17 | 2021-03-19 | 宁夏启元药业有限公司 | Separation method of tetracycline hydrochloride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB799044A (en) * | 1954-01-15 | 1958-07-30 | Bristol Lab Ltd | Certain organic salts of tetracycline and processes for preparing tetracycline hydrochloride and acid and metal salts of tetracycline |
| US3979269A (en) * | 1975-02-25 | 1976-09-07 | DSO "Pharmachim | Method for obtaining tetracyclinehydrochloride |
| CN102993043A (en) * | 2012-12-04 | 2013-03-27 | 天津大学 | Method for preparing high-purity tetracycline hydrochloride |
-
2015
- 2015-11-19 CN CN201510801097.0A patent/CN105294481B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB799044A (en) * | 1954-01-15 | 1958-07-30 | Bristol Lab Ltd | Certain organic salts of tetracycline and processes for preparing tetracycline hydrochloride and acid and metal salts of tetracycline |
| US3979269A (en) * | 1975-02-25 | 1976-09-07 | DSO "Pharmachim | Method for obtaining tetracyclinehydrochloride |
| CN102993043A (en) * | 2012-12-04 | 2013-03-27 | 天津大学 | Method for preparing high-purity tetracycline hydrochloride |
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| CN105294481A (en) | 2016-02-03 |
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