CN107325010A - The safe preparation method and device of a kind of adamantanol - Google Patents
The safe preparation method and device of a kind of adamantanol Download PDFInfo
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- CN107325010A CN107325010A CN201710690149.0A CN201710690149A CN107325010A CN 107325010 A CN107325010 A CN 107325010A CN 201710690149 A CN201710690149 A CN 201710690149A CN 107325010 A CN107325010 A CN 107325010A
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- reaction
- blender
- drive pump
- magnetic drive
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
Abstract
The present invention relates to pharmaceutical synthesis field, the safe preparation method and device of a kind of adamantanol are disclosed, it is scattered by the way that reaction raw materials and the concentrated sulfuric acid are carried out into mixing；The mixed liquor of reaction raw materials and the concentrated sulfuric acid and concentrated nitric acid are pumped into blender using magnetic drive pump；The mixed liquor in blender is pumped into tubular reactor using magnetic drive pump；Collect the reaction solution discharged from tubular reactor and reaction is hydrolyzed；Separation and Extraction and wastewater treatment are carried out to reaction solution, to obtain 3- amino-1-adamantane alcohols.Impurity generation of the present invention is few, and target product yield is high, course of reaction safety, and impure few in waste water, cost for wastewater treatment is substantially reduced.
Description
Technical field
The present invention relates to the safe preparation method and device of pharmaceutical synthesis field, more particularly to a kind of adamantanol.
Background technology
3- amino-1-adamantane alcohols are the intermediate for preparing the multi-medicaments such as treatment Rezulin, domestic and international existing life
The technical matters of 3- amino-1-adamantane alcohols is produced, typically using amantadine or its salt (adamantanamine hydrochloride, Buddha's warrior attendant
Alkanamine sulfate etc.) it is initiation material, after the nitration reaction in sulfonitric mixed acid, hydrolysis, separating-purifying, obtain mesh
Mark the crystallization of product 3- amino-1-adamantane alcohols.In this production preparation process, nitrification of the initiation material in nitration mixture
Reaction is the basis for realizing technology target, directly affects success or failure and the production cost of technology.
There is following major defect in the mixed acid nitrification reaction method of existing synthesis 3- amino-1-adamantane alcohol techniques：
1st, nitration reaction is put into dangerous chemical reaction operation, because nitration reaction is strongly exothermic process, the heat of releasing
Amount raises reaction mass temperature, promotes reaction to accelerate, and more heats are released again.If temperature control is not lived, reaction temperature
Nitric acid chain reaction is produced caused by too high, can cause combustion explosion.Existing nitration reaction is anti-in special kettle type nitration
Answer in device and carry out, hundreds of liters, at most thousands of liters at least per kettle reaction mass useful load.Reaction temperature be normally controlled in 15 DEG C with
Under, 3~5 hours at least reaction time, at most ten a few houres.And during whole nitration reaction, it is necessary to continuously stir and
Logical cooling water temperature.If chance power failure is cut off the water or equipment fault causes radiating not smooth, it is easy to which the material that reacts is rapidly heated
Generation security incident.
2nd, because the reaction mass long period is present in nitration mixture, the strong oxidizing property of the concentrated sulfuric acid can make the product generated
Further occur side reaction, generate impurity.The side reaction that existing nitration reaction method is produced is more, usual target product yield
Only 50%~0%.The more generation of side reaction impurity, also makes the product separating-purifying of later processing operation produce larger life
Produce cost.
3rd, existing nitration reaction temperature need to control to carry out (generally below 15 DEG C) at low temperature, and temperature is too high to make by-product
Thing accelerates, impurity increase.Because reaction mass viscosity is larger under low temperature, and under low temperature, main reaction speed is also relatively slow (especially anti-
Answer later stage main reaction slow), for ease of stirring radiating and promotion late phase reaction speed, sulfuric acid in existing nitration reaction operation
Dosage is larger, usually the 12~15 of initiation material amount times, and the dosage of nitric acid is usually the 12%~25% of sulfuric acid total amount.
So, the wastewater flow rate that reaction mass hydrolysis is produced after terminating is larger (being usually 3~5 times of nitration mixture total amount), is used during processing waste water
In neutralize acid pickle consume alkali (sodium hydroxide etc.) amount it is very big, because impure many in waste water, processing cost is also high.
The content of the invention
The present invention provides a kind of safe preparation method and device of adamantanol, solves the adamantanol production of prior art
The high technical problem of security incident, production cost easily occurs for middle mixed acid nitrification reaction.
The purpose of the present invention is achieved through the following technical solutions：
A kind of safe preparation method of adamantanol, including：
Reaction raw materials and the concentrated sulfuric acid are carried out into mixing to disperse, wherein, the reaction raw materials are amantadine or amantadine
Hydrochloride or amantadine sulfate, the mol ratio of the reaction raw materials and the concentrated sulfuric acid is 1：3 ￣ 1：5；
The mixed liquor of reaction raw materials and the concentrated sulfuric acid and concentrated nitric acid are pumped into blender using magnetic drive pump, wherein, it is described dense
The mol ratio of nitric acid and the concentrated sulfuric acid is 0.08：1~0.15：1；
The mixed liquor in blender is pumped into tubular reactor using magnetic drive pump, wherein, material is in tubular reactor
Residence time be 10s~2min；
Collect the reaction solution discharged from tubular reactor and reaction is hydrolyzed；
Separation and Extraction and wastewater treatment are carried out to reaction solution, to obtain 3- amino-1-adamantane alcohols.
A kind of adamantanol safely prepares device, including the first magnetic drive pump 1, the second magnetic drive pump 2, blender 4, tubular type be anti-
Device 6, hydrolysis agitator 7 are answered, wherein, first magnetic drive pump 1 is connected by magnetic valve 3 with the entrance of the blender 4, described
Second magnetic drive pump 2 is connected by magnetic valve 3 with the entrance of the blender 4, outlet and the tubular reactor 6 of the blender 4
Entrance connection, the outlet of the tubular reactor 6 with it is described hydrolysis agitator 7 connect, first magnetic drive pump 1 with reaction original
Batch can is connected, the concentrated nitric acid storage tank of the second magnetic drive pump 2 connection.
The present invention provides a kind of safe preparation method and device of adamantanol, by the way that reaction raw materials and the concentrated sulfuric acid are carried out
Mixing is scattered；The mixed liquor of reaction raw materials and the concentrated sulfuric acid and concentrated nitric acid are pumped into blender using magnetic drive pump；Utilize magnetic drive pump
Mixed liquor in blender is pumped into tubular reactor；Collect the reaction solution discharged from tubular reactor and be hydrolyzed anti-
Should；Separation and Extraction and wastewater treatment are carried out to reaction solution, to obtain 3- amino-1-adamantane alcohols.Impurity generation of the present invention
Few, target product yield is high, course of reaction safety, and impure few in waste water, cost for wastewater treatment is substantially reduced.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to institute in embodiment
The accompanying drawing needed to use is briefly described, it should be apparent that, drawings in the following description are only some implementations of the present invention
Example, for those of ordinary skill in the art, without having to pay creative labor, can also be obtained according to these accompanying drawings
Obtain other accompanying drawings.
Fig. 1 is a kind of flow chart of the safe preparation method of adamantanol of the embodiment of the present invention；
Fig. 2 is a kind of structure chart for safely preparing device of adamantanol of the embodiment of the present invention.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, it is below in conjunction with the accompanying drawings and specific real
Applying mode, the present invention is further detailed explanation.
As shown in figure 1, be a kind of safe preparation method of adamantanol, including：
Step 101, that reaction raw materials and the concentrated sulfuric acid are carried out into mixing is scattered；
Wherein, the reaction raw materials are amantadine or adamantanamine hydrochloride or amantadine sulfate, the reaction
The mol ratio of raw material and the concentrated sulfuric acid is 1：3 ￣ 1：5；
Step 102, using magnetic drive pump the mixed liquor and concentrated nitric acid of reaction raw materials and the concentrated sulfuric acid are pumped into blender；
Wherein, the mol ratio of the concentrated nitric acid and the concentrated sulfuric acid is 0.08：1~0.15：1；
Step 103, using magnetic drive pump the mixed liquor in blender is pumped into tubular reactor；
Wherein, residence time of the material in tubular reactor is 10s~2min；
Simultaneously reaction is hydrolyzed in step 104, the reaction solution discharged from tubular reactor of collection；
Step 105, separation and Extraction and wastewater treatment are carried out to reaction solution, to obtain 3- amino-1-adamantane alcohols.
Wherein, it can also include before step 102：
Step 102-1, preheated device are preheated to the mixed liquor of reaction raw materials and the concentrated sulfuric acid, and preheating temperature is 40 DEG C
~80 DEG C.
The present invention technique effect be：
1st, due to reaction reagent concentrated nitric acid and reaction raw materials, to immediately enter tubular type after initial contact is mixed in a mixer anti-
Answer in device and react, reaction temperature it is higher but at high temperature the residence time it is very short (only tens of seconds to one, two minutes), main reaction is fast
Speed carries out also Quick stop, and the side reaction of product has little time to occur, therefore impurity generation is few, and target product yield is high, reachable
More than 90%.
2nd, within the same time, the nitration mixture material in blender is no more than 5L, the heated reaction mass in reaction tube
Only hundreds of milliliters, and termination is hydrolyzed in tens of seconds to one, two minutes, therefore nitration reaction process can ensure that safety.
3rd, the sulfuric acid amount added only has the 1/3~1/5 of prior art, and nitric acid throwing amount only has the 1/ of prior art
6~1/10, the wastewater flow rate of generation also only has the 1/3~1/5 of prior art, and impure few in waste water, wastewater treatment into
Originally substantially reduce.
What the embodiment of the present invention additionally provided a kind of adamantanol safely prepares device, as shown in Fig. 2 including the first magnetic force
Pump 1, the second magnetic drive pump 2, blender 4, tubular reactor 6, hydrolysis agitator 7, wherein, first magnetic drive pump 1 passes through electromagnetism
Valve 3 is connected with the entrance of the blender 4, and second magnetic drive pump 2 is connected by magnetic valve 3 with the entrance of the blender 4,
The outlet of the blender 4 is connected with the entrance of tubular reactor 6, and the outlet of the tubular reactor 6 is stirred with the hydrolysis
Device 7 is connected, and first magnetic drive pump 1 is connected with reaction raw materials tank, the concentrated nitric acid storage tank of the second magnetic drive pump 2 connection.
Wherein, tubular reactor 6 is made up of acidproof material or stainless steel tube, and round tube inside diameter is 5mm~15mm, and length of tube is
10m~25m, the shape of reaction tube bends discoid or meander-shaped, and the reaction tube is immersed in the thermal medium of controllable temperature, institute
State and temperature sensor and heating wire are provided with thermal medium.
The periphery of the reaction tube is provided with supersonic generator.
Preheater 5 is provided between the outlet of the blender 4 and the tubular reactor 6.
The volume of the blender is 1L~5L.
The present invention is described in detail above, principle and embodiment party of the specific case used herein to the present invention
Formula is set forth, and the explanation of above example is only intended to the method and its core concept for helping to understand the present invention；Meanwhile, it is right
In those of ordinary skill in the art, according to the thought of the present invention, change is had in specific embodiments and applications
Part, in summary, this specification content should not be construed as limiting the invention.
Claims (7)
1. a kind of safe preparation method of adamantanol, it is characterised in that including：
Reaction raw materials and the concentrated sulfuric acid are carried out into mixing to disperse, wherein, the reaction raw materials are amantadine or amantadine hydrochloric acid
Salt or amantadine sulfate, the mol ratio of the reaction raw materials and the concentrated sulfuric acid is 1：3 ￣ 1：5；
The mixed liquor of reaction raw materials and the concentrated sulfuric acid and concentrated nitric acid are pumped into blender using magnetic drive pump, wherein, the concentrated nitric acid
Mol ratio with the concentrated sulfuric acid is 0.08：1~0.15：1；
The mixed liquor in blender is pumped into tubular reactor using magnetic drive pump, wherein, material stopping in tubular reactor
It is 10s~2min to stay the time；
Collect the reaction solution discharged from tubular reactor and reaction is hydrolyzed；
Separation and Extraction and wastewater treatment are carried out to reaction solution, to obtain 3- amino-1-adamantane alcohols.
2. the safe preparation method of adamantanol according to claim 1, it is characterised in that will react former using magnetic drive pump
The mixed liquor of material and the concentrated sulfuric acid is pumped into before the step in blender with concentrated nitric acid, including：
Preheated device is preheated to the mixed liquor of reaction raw materials and the concentrated sulfuric acid, and preheating temperature is 40 DEG C~80 DEG C.
3. a kind of adamantanol safely prepares device, it is characterised in that including the first magnetic drive pump (1), the second magnetic drive pump (2),
Blender (4), tubular reactor (6), hydrolysis agitator (7), wherein, first magnetic drive pump (1) passes through magnetic valve (3) and institute
The entrance connection of blender (4) is stated, second magnetic drive pump (2) is connected by the entrance of magnetic valve (3) and the blender (4)
Logical, the outlet of the blender (4) is connected with the entrance of tubular reactor (6), the outlet of the tubular reactor (6) with it is described
Agitator (7) connection is hydrolyzed, first magnetic drive pump (1) is connected with reaction raw materials tank, the second magnetic drive pump (2) concentrated nitric acid storage
Batch can is connected.
4. adamantanol according to claim 3 safely prepares device, it is characterised in that tubular reactor (6) is by resistance to
Sour material or stainless steel tube are made, and round tube inside diameter is 5mm~15mm, and length of tube is 10m~25m, the shape bending circle of reaction tube
Plate-like or meander-shaped, the reaction tube are immersed in the thermal medium of controllable temperature, in the thermal medium provided with temperature sensor and
Heating wire.
5. adamantanol according to claim 4 safely prepares device, it is characterised in that the periphery of the reaction tube sets
There is supersonic generator.
6. adamantanol according to claim 3 safely prepares device, it is characterised in that blender (4) go out
Preheater (5) is provided between mouth and the tubular reactor (6).
7. adamantanol according to claim 3 safely prepares device, it is characterised in that the volume of the blender is
1L~5L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710690149.0A CN107325010A (en) | 2017-08-14 | 2017-08-14 | The safe preparation method and device of a kind of adamantanol |
Applications Claiming Priority (1)
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|---|---|---|---|
| CN201710690149.0A CN107325010A (en) | 2017-08-14 | 2017-08-14 | The safe preparation method and device of a kind of adamantanol |
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| CN107325010A true CN107325010A (en) | 2017-11-07 |
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|---|---|---|---|
| CN201710690149.0A Pending CN107325010A (en) | 2017-08-14 | 2017-08-14 | The safe preparation method and device of a kind of adamantanol |
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Cited By (5)
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|---|---|---|---|---|
| CN109824524A (en) * | 2019-03-27 | 2019-05-31 | 浙江信桥生化科技有限公司 | A kind of technique preparing 3- amino-1-adamantane alcohol |
| CN111233644A (en) * | 2020-03-10 | 2020-06-05 | 四川众邦制药有限公司 | Synthesis and extraction method of adamantanone |
| CN111349009A (en) * | 2020-03-10 | 2020-06-30 | 四川众邦制药有限公司 | Synthesis method of 3-hydroxy-1-adamantane carboxylic acid |
| CN112010764A (en) * | 2020-09-18 | 2020-12-01 | 江苏泰洁智邦检测技术有限公司 | Preparation method of 3-hydroxy-1-amantadine transition state intermediate |
| CN112250578A (en) * | 2020-10-26 | 2021-01-22 | 四川众邦制药有限公司 | Method for preparing 1, 3-adamantanediol by using 1-adamantanol as starting raw material |
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Application publication date: 20171107 |