CN106946816A - A kind of preparation method of chloro terramycin - Google Patents
A kind of preparation method of chloro terramycin Download PDFInfo
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- CN106946816A CN106946816A CN201710237313.2A CN201710237313A CN106946816A CN 106946816 A CN106946816 A CN 106946816A CN 201710237313 A CN201710237313 A CN 201710237313A CN 106946816 A CN106946816 A CN 106946816A
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- Prior art keywords
- terramycin
- preparation
- chloro
- methanol
- chloro terramycin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
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- Organic Chemistry (AREA)
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of chloro terramycin, including：1）Methanol is added in equipped with churned mechanically reactor, temperature control adds terramycin at 10 15 DEG C, then into reactor, and N chlorosuccinimides are added after stirring cooling, is sufficiently stirred for reacting 1h, crystal is separated out again after reaction；2）By step 1）In obtained mixture, be injected into filter plant and filter, and washed with methanol, discharging after 30min；3）By step 2）In obtained product, processing is dried by drying equipment.The preparation method of the chloro terramycin of the present invention, reactant N chlorosuccinimides consumption is less, and toxic and side effect is low, improves reaction yield, can reach 95%.The waste residue thus produced is less, with good practicality.
Description
Technical field
The invention belongs to technical field of compound preparation, and in particular to a kind of preparation technology of chloro terramycin.
Background technology
Chloro terramycin is the important intermediate for producing Doxycycline Hyclate, and it is to be made by terramycin by chloro,
And for preparing 11 alpha-chloro -6- methacyclines, and 11 alpha-chloro -6- methacyclines are used to produce Doxycycline Hyclate.
Doxycycline Hyclate is a kind of good antimicrobial, and the medicine is also widely used in veterinary drug in addition, can treat and be caused by a variety of germs
Infection, be mainly used in treatment sensitive bacteria caused by respiratory tract, the urinary tract and infection of biliary tract.The market phase of current fortimicin
To considerable, market demand is very big.
11 alpha-chloro -6,12 hemiketal terramycin（Abbreviation chloro terramycin）
The structure of chloro terramycin is as shown in above formula.The production technology of usual chloro terramycin is：Terramycin is added without water beetle
In alcohol, low temperature stirring is lower to add acetochloroanilide, reaction generation chloro terramycin and antifebrin, chloro terramycin Cheng Jing
Body is separated out, and is filtered out chloro terramycin Mother liquor and is reclaimed methanol, the technique toxic and side effect is big, environmental hazard effect is big, reaction yield
It is low, produce waste residue more.
The content of the invention
Goal of the invention：For the deficiencies in the prior art, it is an object of the invention to provide a kind of chloro terramycin
Preparation method, toxic and side effect is low, improves reaction yield.
Technical scheme：In order to realize foregoing invention purpose, the technical solution adopted by the present invention is：
A kind of preparation method of chloro terramycin, comprises the following steps：
1）Methanol is added in equipped with churned mechanically reactor, temperature control is at 10-15 DEG C, then adds into reactor terramycin,
N- chlorosuccinimides are added after stirring cooling, are sufficiently stirred for reacting 1h, crystal is separated out again after reaction；
2）By step 1）In obtained mixture, be injected into filter plant and filter, and washed with methanol, gone out after 30min
Material；
3）By step 2）In obtained product, processing is dried by drying equipment.
Step 2）In, filter plant can be Vacuum filtration device or industrial centrifugal machine, plate and frame filter press, circle
Cylinder filter press etc..
Step 3）In, drying equipment includes vacuum drying oven, convection oven, pneumatic conveying dryer etc..
Step 1）In, raw material proportioning：Terramycin 100-150kg, methanol 800-1200L, N- chlorosuccinimide 30-
50kg。
Step 3）In, 70-85 DEG C of temperature dries 1h, obtains chloro terramycin dry product.
Beneficial effect, compared with prior art, the preparation method of chloro terramycin of the invention, reactant N- chloros fourth two
Acid imide consumption is less, and toxic and side effect is low, improves reaction yield, can reach 95%.The waste residue thus produced is less, has
Good practicality.
Embodiment
With reference to specific embodiment, the present invention is described further.
Embodiment 1
A kind of preparation method of chloro terramycin, comprises the following steps：
1）500mL methanol is added to 1000mL reactor, temperature control adds the native mould of 60g into reactor at 10-15 DEG C
Element is stirred；It is sufficiently stirred for after 1h, is cooled to 5 DEG C, add 30g N- chlorosuccinimides, stirs 1h；
2）Above-mentioned material filtering is separated, and washed with methanol, is discharged after suction filtration 30min；
3）By step 2）Obtained product, processing is dried by drying box, finally obtained fortimicin important intermediate chlorine
For terramycin 58.83g, yield 98%.
Embodiment 2
A kind of preparation method of chloro terramycin, comprises the following steps：
1）5L methanol is added to 10L reactor, temperature control is at 10-15 DEG C, and the terramycin that 0.6kg is added into reactor enters
Row stirring；It is sufficiently stirred for after 1h, is cooled to 0 DEG C, add 0.3kg N- chlorosuccinimides, stirs 1h；
2）By step 1）It is injected into centrifuge and carries out getting rid of material, and washed with methanol, is discharged after getting rid of material 30min；
3）By step 2）Obtained product, by air dry oven drying process, is finally made fortimicin important intermediate chlorine
For terramycin 0.57kg, yield 95%.
Embodiment 3
A kind of preparation method of chloro terramycin, comprises the following steps：
1）500L methanol is added to 1000L reactor, temperature control adds the native mould of 60kg into reactor at 10-15 DEG C
Element is stirred, and is sufficiently stirred for after 1h, is cooled to 0 DEG C of addition 30kg N- chlorosuccinimides, is stirred 1h；
2）By step 1）It is injected into filter press and carries out press filtration, is discharged after press filtration 1h；
3）By step 2）Obtained product, by Air Dried System drying process, is finally made fortimicin important intermediate
Chloro terramycin 59.33kg, yield 98.9%.
Claims (5)
1. a kind of preparation method of chloro terramycin, it is characterised in that comprise the following steps：
1）Methanol is added in equipped with churned mechanically reactor, temperature control is at 10-15 DEG C, then adds into reactor terramycin,
N- chlorosuccinimides are added after stirring cooling, are sufficiently stirred for reacting 1h, crystal is separated out again after reaction；
2）By step 1）In obtained mixture, be injected into filter plant and filter, and washed with methanol, gone out after 30min
Material；
3）By step 2）In obtained product, processing is dried by drying equipment.
2. the preparation method of chloro terramycin according to claim 1, it is characterised in that step 2）In, filter plant is
Vacuum filtration device, industrial centrifugal machine, plate and frame filter press, cylinder filter press.
3. the preparation method of chloro terramycin according to claim 1, it is characterised in that step 3）In, drying equipment bag
Include vacuum drying oven, convection oven, pneumatic conveying dryer.
4. the preparation method of chloro terramycin according to claim 1, it is characterised in that step 1）In, raw material proportioning：Soil
Mycin 100-150kg, methanol 800-1200L, N- chlorosuccinimide 30-50kg.
5. the preparation method of chloro terramycin according to claim 1, it is characterised in that step 3）In, temperature 70-85
DEG C, 1h is dried, chloro terramycin dry product is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710237313.2A CN106946816A (en) | 2017-04-12 | 2017-04-12 | A kind of preparation method of chloro terramycin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710237313.2A CN106946816A (en) | 2017-04-12 | 2017-04-12 | A kind of preparation method of chloro terramycin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106946816A true CN106946816A (en) | 2017-07-14 |
Family
ID=59474536
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710237313.2A Pending CN106946816A (en) | 2017-04-12 | 2017-04-12 | A kind of preparation method of chloro terramycin |
Country Status (1)
| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111393319A (en) * | 2020-04-24 | 2020-07-10 | 山东国邦药业有限公司 | Preparation method of oxytetracycline chloride |
| CN115043751A (en) * | 2022-08-16 | 2022-09-13 | 山东国邦药业有限公司 | Synthesis method of N-chloro-oxytetracycline |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1370318A (en) * | 1970-12-28 | 1974-10-16 | Rachelle Lab Italia Spa | Manufacture of 6-methylenetetracyclines |
-
2017
- 2017-04-12 CN CN201710237313.2A patent/CN106946816A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1370318A (en) * | 1970-12-28 | 1974-10-16 | Rachelle Lab Italia Spa | Manufacture of 6-methylenetetracyclines |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111393319A (en) * | 2020-04-24 | 2020-07-10 | 山东国邦药业有限公司 | Preparation method of oxytetracycline chloride |
| CN111393319B (en) * | 2020-04-24 | 2023-03-28 | 山东国邦药业有限公司 | Preparation method of oxytetracycline chloride |
| CN115043751A (en) * | 2022-08-16 | 2022-09-13 | 山东国邦药业有限公司 | Synthesis method of N-chloro-oxytetracycline |
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Application publication date: 20170714 |