CN108276333A - A kind of preparation process and its device of carbidopa midbody acridine - Google Patents
A kind of preparation process and its device of carbidopa midbody acridine Download PDFInfo
- Publication number
- CN108276333A CN108276333A CN201810385981.4A CN201810385981A CN108276333A CN 108276333 A CN108276333 A CN 108276333A CN 201810385981 A CN201810385981 A CN 201810385981A CN 108276333 A CN108276333 A CN 108276333A
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- CN
- China
- Prior art keywords
- acridine
- pipeline
- carbidopa
- midbody
- mixer
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D219/00—Heterocyclic compounds containing acridine or hydrogenated acridine ring systems
- C07D219/02—Heterocyclic compounds containing acridine or hydrogenated acridine ring systems with only hydrogen, hydrocarbon or substituted hydrocarbon radicals, directly attached to carbon atoms of the ring system
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D273/00—Heterocyclic compounds containing rings having nitrogen and oxygen atoms as the only ring hetero atoms, not provided for by groups C07D261/00 - C07D271/00
- C07D273/01—Heterocyclic compounds containing rings having nitrogen and oxygen atoms as the only ring hetero atoms, not provided for by groups C07D261/00 - C07D271/00 having one nitrogen atom
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention provides a kind of preparation processes of carbidopa midbody acridine, include the following steps：A. water and ammonium hydroxide, stirring cooling are added into mixing liquid storage tank；B. it adds acetone and is made into mixed liquor, cool down；C. dichloromethane and sodium hypochlorite are cooled down；D. make three kinds of mixed liquor, dichloromethane, sodium hypochlorite liquid, first pass through mixer, then flow into layering tank after pipeline reactor hybrid reaction, lower layer's organic phase is product.The present invention also provides a kind of preparation facilities of carbidopa midbody acridine, enable reactant under the conditions of constant temperature using pipeline reactor, fast reaction, it solves acridine to react at low temperature slowly, the labile problem of high temperature, operating environment greatly improves, shorten the process time, it improves work efficiency, reduces energy consumption, with good economic efficiency and social benefit.
Description
Technical field
The present invention relates to a kind of preparation processes and its device of carbidopa midbody acridine, belong to the field of chemical synthesis skill
Art field.
Background technology
Carbidopa is periphery decarboxylase inhibitors, is not easily accessible maincenter, only periphery levodopa is inhibited to be converted into DOPA
Amine makes the effect of levodopa content increases, improves the concentration of intracerebral dopamine, enhance levodopa in cycle, is left-handed more
Bar important adjuvant drug, for parkinsonism caused by a variety of causes.
Acridine is to prepare one of important intermediate of carbidopa, and reaction process is：
Domestic at present and production carbidopa producer is less in the world, conventional preparation techniques are to be added in a kettle mostly
Acetone, ammonium hydroxide, dichloromethane, water, then cool down, and are added with stirring sodium hypochlorite, after a certain period of time, stratification has for stirring
Machine layer is directly used in react in next step.
The disadvantage is that：
Acridine property is unstable, is extremely easy in decomposition, and low-temp reaction is slow, and temperature Gao Shiyi is decomposed.Traditional handicraft is amplified in production
Afterwards, the time is longer, temperature control is difficult and complex for operation step, and acridine decomposes seriously in the process, and content reduces.Therefore in order to
Shorten the process time and improve reaction efficiency and make up the market vacancy, develops the process unit being simple to operate and friendly to environment very
It is necessary.
Invention content
The object of the present invention is to provide a kind of preparation processes of carbidopa midbody acridine, the technical solution adopted is that：
The preparation process it is characterized by comprising the following steps：
A. the water and ammonium hydroxide of dosage are added into mixing liquid storage tank, obtains ammonia spirit, stirring cooling；
B. the acetone for adding dosage is made into mixed liquor, cooling, for use；
C. dichloromethane and sodium hypochlorite are cooled down, for use；
D. dnockout pumps are opened, makes three kinds of mixed liquor, dichloromethane, sodium hypochlorite liquid under certain flow, first passes through mixed
Clutch is pre-mixed, then is flowed into acridine after pipeline reactor hybrid reaction and be layered tank, and lower layer's organic phase is product acridine solution.
A kind of preparation process of the carbidopa midbody acridine, it is characterised in that：Ammonia spirit contains in step A
Amount is 0.8-3.0% (w/w), is cooled to 5-20 DEG C.
A kind of preparation process of the carbidopa midbody acridine, it is characterised in that：It is cooled to -10-15 in step B
℃。
A kind of preparation process of the carbidopa midbody acridine, it is characterised in that：In step C dichloromethane and time
Sodium chlorate is cooled to -10-15 DEG C.
A kind of preparation process of the carbidopa midbody acridine, it is characterised in that：Flow quantity is mixed in step D is
1.3-3.7m3/ h and dichloromethane flow are 2.1-4.8m3/ h, sodium hypochlorite flow are 0.7-2.5m3/h。
It is another object of the present invention to additionally provide a kind of preparation work that can realize above-mentioned carbidopa midbody acridine
The device of skill, the device include sodium hypochlorite storage tank 1, dichloromethane storage tank 2, mixing liquid storage tank 3, the first dnockout pumps 4, second dozens
Material pump 5, third dnockout pumps 6, first flowmeter 7, second flowmeter 8, third flowmeter 9, mixer 10, pipeline reactor 11,
Stratification tank 12；1 pot bottom discharge port of sodium hypochlorite storage tank is connected with 4 feed inlet of the first dnockout pumps by pipeline, dichloromethane
2 bottom discharge mouth of alkane storage tank is connected with 5 feed inlet of the second dnockout pumps by pipeline, and 3 bottom discharge mouth of liquid storage tank and third are mixed
6 feed inlet of dnockout pumps is connected by pipeline, and 4 discharge port of the first dnockout pumps, 5 discharge port of the second dnockout pumps, third dnockout pumps 6 discharge
Mouth is connected by pipeline with the feed inlet on 10 top of mixer, and the pipeline that the first dnockout pumps 4 are connected with mixer 10 is equipped with first
Flowmeter 7, the pipeline that the second dnockout pumps 5 are connected with mixer 10 are equipped with second flowmeter 8, third dnockout pumps 6 and mixer 10
Connected pipeline is equipped with third flowmeter 9, and 10 discharge port of mixer is connected with the feed inlet of pipeline reactor 11, pipeline reactor
11 discharge ports are connected with 12 feed inlet of stratification tank.
The pipeline reactor 11 is chuck riser reactor, and reactor standpipe number is 3, and connection type is string
Connection.
The pipeline reactor feed inlet 13 is connected with 10 discharge port of mixer.
The pipeline reactor discharge port 14 is connected with 12 feed inlet of stratification tank.
The pipeline reactor chuck feed inlet 15 is connected with brine ice feeding pipe, pipeline reactor chuck discharge port
16 are connected with cryosel water loop.
11 inner stuffing 18 of pipeline reactor is fixed anti-corrosion precision filler.
The chuck riser reactor is using high-quality stainless steel (304,316L) or specialty metal --- titanium (TA2) etc.
Material precision manufactureing, surfaces externally and internally carry out fine polishing treatment.This reactor jacket conveys heat transfer medium, and inside reactor is solid
Fixed pattern anti-corrosion precision filler is conveyed feed liquid into inside reactor by dnockout pumps, and reaction material liquid passes through reactor precision filler
It is sufficiently mixed reaction, to achieve the purpose that quick, low temperature preparation acridine.This reactor can need to increase according to production series connection instead
Device number is answered, can also be needed to increase parallel pipeline according to production.
The invention has the advantages that：
Present invention design is simple, scientific and reasonable, enables reactant under the conditions of constant temperature using pipeline reactor, quickly anti-
It answers, solves acridine and react at low temperature slowly, the labile problem of high temperature, operating environment greatly improves, and shortens the process time,
It improves work efficiency, reduces energy consumption, with good economic efficiency and social benefit.
Description of the drawings
Fig. 1 is schematic structural view of the invention；
Fig. 2 is inventive pipeline structure of reactor schematic diagram；
In figure：1, sodium hypochlorite storage tank；2, dichloromethane storage tank；3, liquid storage tank is mixed；4 first dnockout pumps；5 second dnockouts
Pump；6 third dnockout pumps；7, first flowmeter；8, second flowmeter；9, third flowmeter；10, mixer；11, pipe reaction
Device；12, stratification tank；13, pipeline reactor feed inlet；14, pipeline reactor discharge port；15, pipeline reactor chuck into
Material mouth；16, pipeline reactor chuck discharge port；17, pipeline reactor chuck；18, inner stuffing.
Specific implementation mode
The invention will now be further described with reference to specific embodiments, the advantages and features of the present invention will be with description and
It is apparent.But examples are merely exemplary for these, and it is not intended to limit the scope of the present invention in any way.People in the art
Member it should be understood that without departing from the spirit and scope of the invention can to the details of technical solution of the present invention and form into
Row modifications or substitutions, but these modifications and replacement are each fallen in protection scope of the present invention.
Embodiment 1
A kind of preparation process of carbidopa midbody acridine, includes the following steps：
A. the water and ammonium hydroxide of dosage are added into mixing liquid storage tank, it is 1.5% ammonia spirit, cooling to obtain content (W/W)
To 10 DEG C.
B. the acetone that dosage is added is made into mixed liquor, is cooled to 5 DEG C, for use.
C. dichloromethane and sodium hypochlorite are down to 5 DEG C.
D. dnockout pumps are opened, control mixing flow quantity is 2.7m3/ h, dichloromethane flow are 3.0m3/ h, sodium hypochlorite stream
Amount is in 1.5m3/h.Three kinds of liquid first pass through mixer premixing, then acridine layering is flowed into after pipeline reactor hybrid reaction
Tank, lower layer's organic phase are product acridine solution.The acridine content prepared by the technique is higher, stable quality.
Embodiment 2
A kind of preparation process of carbidopa midbody acridine, includes the following steps：
A. the water and ammonium hydroxide of dosage are added into mixing liquid storage tank, it is 1.0% ammonia spirit, cooling to obtain content (W/W)
To 7.0 DEG C.
B. the acetone that dosage is added is made into mixed liquor, is cooled to 3 DEG C, for use.
C. dichloromethane and sodium hypochlorite are down to -2.0 DEG C.
D. dnockout pumps are opened, control mixing flow quantity is 2.0m3/ h, dichloromethane flow are 2.5m3/ h, sodium hypochlorite stream
Amount is in 1.2m3/h.Three kinds of liquid first pass through mixer premixing, then acridine layering is flowed into after pipeline reactor hybrid reaction
Tank, lower layer's organic phase are product acridine solution.The acridine content prepared by the technique is higher, stable quality.
Embodiment 3
A kind of preparation process of carbidopa midbody acridine, includes the following steps：
A. toward mixed liquor tank water and ammonium hydroxide, it is 2.5% ammonia spirit to obtain content (W/W), is cooled to 15.0 DEG C.
B. the acetone that dosage is added is made into mixed liquor, is cooled to -2.0 DEG C, for use.
C. dichloromethane and sodium hypochlorite are down to 10 DEG C.
D. dnockout pumps are opened, control mixing flow quantity is 3.0m3/ h, dichloromethane flow are 4.0m3/ h, sodium hypochlorite stream
Amount is in 2.0m3/h.Three kinds of liquid first pass through mixer premixing, then acridine layering is flowed into after pipeline reactor hybrid reaction
Tank, lower layer's organic phase are product acridine solution.The acridine content prepared by the technique is higher, stable quality.
Embodiment 4
A kind of device of the preparation of carbidopa midbody acridine, the device include sodium hypochlorite storage tank 1, dichloromethane storage
Tank 2, mixing liquid storage tank 3, the first dnockout pumps 4, the second dnockout pumps 5, third dnockout pumps 6, first flowmeter 7, second flowmeter 8,
Third flowmeter 9, mixer 10, pipeline reactor 11, stratification tank 12；1 pot bottom discharge port of sodium hypochlorite storage tank and
One dnockout pumps, 4 feed inlet is connected by pipeline, and 2 bottom discharge mouth of dichloromethane storage tank and 5 feed inlet of the second dnockout pumps pass through pipe
Road is connected, and mixing 3 bottom discharge mouth of liquid storage tank is connected with 6 feed inlet of third dnockout pumps by pipeline, the discharging of the first dnockout pumps 4
Mouth, 5 discharge port of the second dnockout pumps, 6 discharge port of third dnockout pumps are connected by pipeline with the feed inlet on 10 top of mixer, and first
The pipeline that dnockout pumps 4 are connected with mixer 10 is equipped with first flowmeter 7, and the pipeline that the second dnockout pumps 5 are connected with mixer 10 is set
Have a second flowmeter 8, the pipeline that third dnockout pumps 6 are connected with mixer 10 is equipped with third flowmeter 9,10 discharge port of mixer with
The feed inlet of pipeline reactor 11 is connected, and 11 discharge port of pipeline reactor is connected with 12 feed inlet of stratification tank.
The pipeline reactor 11 is chuck riser reactor, and reactor standpipe number is 3, and connection type is string
Connection.
The pipeline reactor feed inlet 13 is connected with 10 discharge port of mixer.
The pipeline reactor discharge port 14 is connected with 12 feed inlet of stratification tank.
The pipeline reactor chuck feed inlet 15 is connected with brine ice feeding pipe, pipeline reactor chuck discharge port
16 are connected with cryosel water loop.
11 inner stuffing 18 of pipeline reactor is fixed anti-corrosion precision filler.
The chuck riser reactor carries out essence using high-quality stainless steel (304,316L) precision manufactureing, surfaces externally and internally
Fine polishing light processing.
Claims (9)
1. a kind of preparation process of carbidopa midbody acridine, which is characterized in that include the following steps：
A. the water and ammonium hydroxide of dosage are added into mixing liquid storage tank, obtains ammonia spirit, stirring cooling；
B. the acetone for adding dosage is made into mixed liquor, cooling, for use；
C. dichloromethane and sodium hypochlorite are cooled down, for use；
D. dnockout pumps are opened, makes three kinds of mixed liquor, dichloromethane, sodium hypochlorite liquid under certain flow, first passes through mixer
Premixing, then flow into acridine after pipeline reactor hybrid reaction and be layered tank, lower layer's organic phase is product acridine solution.
2. a kind of preparation process of carbidopa midbody acridine according to claim 1, it is characterised in that：In step A
The content of ammonia spirit is 0.8-3.0% (w/w), is cooled to 5-20 DEG C.
3. a kind of preparation process of carbidopa midbody acridine according to claim 1, it is characterised in that：In step B
It is cooled to -10-15 DEG C.
4. a kind of preparation process of carbidopa midbody acridine according to claim 1, it is characterised in that：In step C
Dichloromethane and sodium hypochlorite are cooled to -10-15 DEG C.
5. a kind of preparation process of carbidopa midbody acridine according to claim 1, it is characterised in that：In step D
Mixing flow quantity is 1.3-3.7m3/ h and dichloromethane flow are 2.1-4.8m3/ h, sodium hypochlorite flow are 0.7-2.5m3/h。
6. a kind of device of the preparation of carbidopa midbody acridine, it is characterised in that：The device includes sodium hypochlorite storage tank
(1), dichloromethane storage tank (2), mixing liquid storage tank (3), the first dnockout pumps (4), the second dnockout pumps (5), third dnockout pumps (6),
Mixer (10), pipeline reactor (11), stratification tank (12), first flowmeter (7), second flowmeter (8), third flow
It counts (9)；Sodium hypochlorite storage tank (1) bottom discharge mouth is connected with the first dnockout pumps (4) feed inlet by pipeline, dichloromethane storage tank
(2) bottom discharge mouth is connected with the second dnockout pumps (5) feed inlet by pipeline, mixes liquid storage tank (3) bottom discharge mouth and third
Dnockout pumps (6) feed inlet is connected by pipeline, and the first dnockout pumps (4) discharge port, the second dnockout (5) pump out material mouth, third dnockout
Pump (6) discharge port is connected by pipeline with the feed inlet on mixer (10) top, and the first dnockout pumps (4) are connected with mixer (10)
Pipeline be equipped with first flowmeter (7), the pipeline that the second dnockout pumps (5) are connected with mixer (10) equipped with second flowmeter (8),
The pipeline that third dnockout pumps (6) are connected with mixer (10) is equipped with third flowmeter (9), and mixer (10) discharge port and pipeline are anti-
The feed inlet (13) of device is answered to be connected, the pipeline reactor discharge port (14) is connected with stratification tank (12) feed inlet.
7. a kind of device of the preparation of carbidopa midbody acridine according to claim 6, it is characterised in that：The pipeline
Reactor (11) is chuck riser reactor, and reactor standpipe number is 1-10, and connection type can be string as needed
Connection, parallel connection.
8. a kind of device of the preparation of carbidopa midbody acridine according to claim 6, it is characterised in that：The pipeline
Reactor jacket feed inlet (15) is connected with brine ice feeding pipe, pipeline reactor chuck discharge port (16) and cryosel water loop
It is connected.
9. a kind of device of the preparation of carbidopa midbody acridine according to claim 6, it is characterised in that：The pipeline
Reactor (11) inner stuffing (18) is fixed anti-corrosion precision filler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810385981.4A CN108276333A (en) | 2018-04-26 | 2018-04-26 | A kind of preparation process and its device of carbidopa midbody acridine |
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| CN201810385981.4A CN108276333A (en) | 2018-04-26 | 2018-04-26 | A kind of preparation process and its device of carbidopa midbody acridine |
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| CN201810385981.4A Pending CN108276333A (en) | 2018-04-26 | 2018-04-26 | A kind of preparation process and its device of carbidopa midbody acridine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029641A (en) * | 2020-09-10 | 2020-12-04 | 广州市金因源生物技术有限公司 | Fermentation device |
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| CN112029641A (en) * | 2020-09-10 | 2020-12-04 | 广州市金因源生物技术有限公司 | Fermentation device |
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