CN108341765A - A kind of preparation method of the high-purity Sulpiride of environmental protection - Google Patents
A kind of preparation method of the high-purity Sulpiride of environmental protection Download PDFInfo
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- CN108341765A CN108341765A CN201810315585.4A CN201810315585A CN108341765A CN 108341765 A CN108341765 A CN 108341765A CN 201810315585 A CN201810315585 A CN 201810315585A CN 108341765 A CN108341765 A CN 108341765A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/04—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
- C07D207/08—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hydrocarbon radicals, substituted by hetero atoms, attached to ring carbon atoms
- C07D207/09—Radicals substituted by nitrogen atoms, not forming part of a nitro radical
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention discloses a kind of preparation methods of the high-purity Sulpiride of environmental protection, include the following steps：It is prepared by crude product；Bamboo charcoal activation；Wherein during bamboo charcoal activation, bamboo powder is fermented using EM bacterium solutions, dry, pulverize, immerse in sodium hydroxide solution and stand, filter, it is dry, it is sent into the activation of vacuum tank high temperature, is washed to being in neutrality, be dry, pulverize, obtain Activated Bamboo；During purifying crude, absolute ethyl alcohol is added into crude product for purifying crude, in 80 100 DEG C of reflux of temperature, 02 DEG C are cooled to, filtering, a concentration of 80 95wt% ethanol solutions are added, in 80 100 DEG C of reflux of temperature, Activated Bamboo is added and continues to flow back, is ultrasonically treated, filtering, crystallization, vacuum drying obtain the high-purity Sulpiride of environmental protection.Product purity and high income of the present invention, preparation process is simple, and preparation process organic matter dosage is few, and in addition ethyl alcohol recycling is easy and repeats to utilize in waste, can reduce the waste to resource and the pollution to environment, safety and environmental protection.
Description
Technical field
The present invention relates to Sulpiride preparing technical field more particularly to a kind of preparation methods of the high-purity Sulpiride of environmental protection.
Background technology
Sulpiride is also Lin-1403, oxazepan, ekilid or Sulpiride, is benzamides antipsychotic drug, can be used for essence
Depressive state, symptomatic psychosis, neurotic depression and the hypochondriasis state of refreshing Split disease, alcoholic psychosis, intelligence hair
Educate not entirely with personality disorder, senile phychosis, especially have it is indifferent, shrink back, be numb, is depressed, illusion, suspection and vain hope
Etc. symptoms patient, and be central antiemetic, have very strong antiemetic effect.Sulpiride synthetic method has more documents at present
Report, is mostly prepared by solvent of ethylene glycol, time-consuming and laborious again by washing to obtain the final product, but in preparation process after filtering, and
And the largely sewage containing organic matter is generated, and the purity of gained Sulpiride product is not also high.
Invention content
The present invention proposes a kind of preparation method of the high-purity Sulpiride of environmental protection, prepared by product purity and high income of the present invention
Simple for process, preparation process organic matter dosage is few, and in addition ethyl alcohol recycling is easy and repeats to utilize in waste, can reduce to money
The waste in source and pollution to environment, safety and environmental protection.
The present invention proposes a kind of preparation method of the high-purity Sulpiride of environmental protection, includes the following steps：
It is prepared by S1, crude product
2- methoxyl group -5- sulfamoylbenzoic acids methyl esters, -2 aminomethyl tetrahydro pyrrolidine of N- ethyls are sent into reaction vessel
In, glycerine is added, in 90-95 DEG C of reaction of temperature under nitrogen protection, water is added to stir, is cooled to room temperature, stopping is passed through nitrogen, continues
It is cooled to 0-2 DEG C, is stood, is filtered, it is dry, obtain crude product；
S2, bamboo charcoal activation
Bamboo powder is fermented using EM bacterium solutions, dry, pulverize, immerse in sodium hydroxide solution and stand, filter, it is dry, it is sent into
Vacuum tank high temperature activates, and washs to being in neutrality, dry, pulverize, obtain Activated Bamboo；
S3, purifying crude
Absolute ethyl alcohol is added into crude product, in 80-100 DEG C of reflux of temperature, is cooled to 0-2 DEG C, filtering is added a concentration of
80-95wt% ethanol solutions are added Activated Bamboo and continue to flow back, be ultrasonically treated in 80-100 DEG C of reflux of temperature, filtering, crystallization,
Vacuum drying obtains the high-purity Sulpiride of environmental protection.
Wherein in bamboo charcoal activation, bamboo powder can effectively remove internal impurity after the fermentation of EM bacterium solutions, and gap of ventilating contains
Amount is high, and vacuum calcining after being handled further across sodium hydroxide alkalization, inner pore structure is flourishing, and product activity is high, absorption speed
Degree is fast, and adsorption capacity is high.
Preferably, in S1,2- methoxyl group -5- sulfamoylbenzoic acids methyl esters, -2 aminomethyl tetrahydro pyrrolidine of N- ethyls
Weight ratio 2-4：1-2.
Preferably, in S1, in 90-95 DEG C of reaction of temperature, reaction time 2-4h under nitrogen protection.
Preferably, in S2, the weight ratio of bamboo powder and EM bacterium solutions is 10：The pH value 3.5-4.5 of 1-2, EM bacterium solution.
Preferably, in S2, it is sent into the activation of vacuum tank high temperature, first in 800-840 DEG C of heat preservation 20-40min of temperature, so
Room temperature is cooled to the speed of 0.2-0.8 DEG C/min afterwards.
Preferably, in S3,100-200 parts of absolute ethyl alcohols are added by weight into 10-20 parts of crude products, in temperature 80-
100 DEG C of reflux 5-15min, are cooled to 0-2 DEG C, and 100-140 parts of a concentration of 80-95wt% ethanol solutions are added, in temperature in filtering
80-100 DEG C of reflux 2-5min.
Preferably, in S3, crude product, Activated Bamboo weight ratio be 5-10：1-2.
Preferably, in S3, Activated Bamboo is added and continues the 10-20min that flows back, is ultrasonically treated 10-40min, supersonic frequency
For 20-30KHz.
Preferably, in S3, in process of vacuum drying, drying temperature is 50-60 DEG C, vacuum degree 0.01-0.05MPa.
In the present invention, 2- methoxyl groups -5- sulfamoylbenzoic acids methyl esters is with -2 aminomethyl tetrahydro pyrrolidine of N- ethyls in nitrogen
It is reacted under gas shielded and Sulpiride crude product is made, when being purified by absolute ethyl alcohol and ethanol water, high temperature reflux and crystallisation by cooling
It is combined, and rationally control proportioning and response parameter, on the one hand not only degree height is precipitated in crystal, and impurity content is few, on the other hand
The usage amount of absolute ethyl alcohol and ethanol water is few, can reduce the waste to resource and the pollution to environment, in addition in waste
The recycling of ethyl alcohol is easy and repeatable utilization, greatly reduces cost input；Further cooperation Activated Bamboo high temperature reflux processing,
The adsorption activity of Activated Bamboo is high, and internal a large amount of pore structure, cooperation are ultrasonically treated, can to various sizes of impurity into
Row absorption and fixed, obtains the Sulpiride purified product that total impurities are no more than 0.08%, and this method not only high income, purity
Also high.
Specific implementation mode
Embodiment 1
A kind of preparation method of the high-purity Sulpiride of environmental protection, includes the following steps：
It is prepared by S1, crude product
10g 2- methoxyl group -5- sulfamoylbenzoic acids methyl esters, -2 aminomethyl tetrahydro pyrrolidine of 5g N- ethyls are sent into anti-
It answers in container, 104g glycerine is added, stirs 24min in 91 DEG C of reaction 2h of temperature, addition 210g water under nitrogen protection, is cooled to room
Temperature, stopping are passed through nitrogen, continue to be cooled to 0 DEG C, stand 11min, filter, dry, obtain crude product；
S2, bamboo charcoal activation
10g bamboo powders are fermented 11 days using 1.2g EM bacterium solutions, dry, pulverize, immerse a concentration of 1.2mol/L sodium hydroxides
21h is stood in solution, is filtered, it is dry, it is sent into vacuum tank in 802 DEG C of heat preservation 22min of temperature, is dropped with the speed of 0.2 DEG C/min
It warms to room temperature, washs to being in neutrality, dry, pulverize, obtain Activated Bamboo；
S3, purifying crude
110g absolute ethyl alcohols are added into 11g crude products, in 82 DEG C of reflux 6min of temperature, is cooled to 0 DEG C, filters, be added
A concentration of 81wt% ethanol solutions of 105g are added 2.3g Activated Bamboos and continue the 11min that flows back, surpass in 82 DEG C of reflux 2min of temperature
Sonication 12min, supersonic frequency 21KHz, filtering, crystallization, vacuum drying, drying temperature are 51 DEG C, and vacuum degree is
0.012MPa obtains the high-purity Sulpiride of environmental protection；The present embodiment yield is 89.2%, purity 99.2%.
Embodiment 2
A kind of preparation method of the high-purity Sulpiride of environmental protection, includes the following steps：
It is prepared by S1, crude product
20g 2- methoxyl group -5- sulfamoylbenzoic acids methyl esters, -2 aminomethyl tetrahydro pyrrolidine of 10g N- ethyls are sent into
In reaction vessel, 135g glycerine is added, stirs 38min in 94 DEG C of reaction 4h of temperature, addition 380g water under nitrogen protection, is cooled to
Room temperature, stopping are passed through nitrogen, continue to be cooled to 2 DEG C, stand 18min, filter, dry, obtain crude product；
S2, bamboo charcoal activation
10g bamboo powders are fermented 19 days using 2g EM bacterium solutions, dry, pulverize, it is molten to immerse a concentration of 1.4mol/L sodium hydroxides
28h is stood in liquid, is filtered, it is dry, it is sent into vacuum tank in 825 DEG C of heat preservation 36min of temperature, is cooled down with the speed of 0.7 DEG C/min
To room temperature, washs to being in neutrality, dry, pulverize, obtain Activated Bamboo；
S3, purifying crude
182g absolute ethyl alcohols are added into 19g crude products, in 94 DEG C of reflux 13min of temperature, is cooled to 2 DEG C, filters, be added
A concentration of 94wt% ethanol solutions of 136g are added 4g Activated Bamboos and continue the 18min that flows back, ultrasound in 96 DEG C of reflux 4min of temperature
36min, supersonic frequency 27KHz are handled, filtering, crystallization, vacuum drying, drying temperature is 56 DEG C, vacuum degree 0.05MPa,
Obtain the high-purity Sulpiride of environmental protection；The present embodiment yield is 89.3%, purity 99.4%.
Embodiment 3
A kind of preparation method of the high-purity Sulpiride of environmental protection, includes the following steps：
It is prepared by S1, crude product
14g 2- methoxyl group -5- sulfamoylbenzoic acids methyl esters, -2 aminomethyl tetrahydro pyrrolidine of 8g N- ethyls are sent into anti-
It answers in container, 120g glycerine is added, stirs 32min in 93 DEG C of reaction 3h of temperature, addition 320g water under nitrogen protection, is cooled to room
Temperature, stopping are passed through nitrogen, continue to be cooled to 1 DEG C, stand 16min, filter, dry, obtain crude product；
S2, bamboo charcoal activation
10g bamboo powders are fermented 16 days using 1.4g EM bacterium solutions, dry, pulverize, immerse a concentration of 1.3mol/L sodium hydroxides
26h is stood in solution, is filtered, it is dry, it is sent into vacuum tank in 825 DEG C of heat preservation 32min of temperature, is dropped with the speed of 0.4 DEG C/min
It warms to room temperature, washs to being in neutrality, dry, pulverize, obtain Activated Bamboo；
S3, purifying crude
160g absolute ethyl alcohols are added into 16g crude products, in 92 DEG C of reflux 10min of temperature, is cooled to 1 DEG C, filters, be added
A concentration of 88wt% ethanol solutions of 120g are added 3g Activated Bamboos and continue the 15min that flows back, ultrasound in 92 DEG C of reflux 4min of temperature
32min, supersonic frequency 28KHz are handled, filtering, crystallization, vacuum drying, drying temperature is 55 DEG C, vacuum degree 0.03MPa,
Obtain the high-purity Sulpiride of environmental protection；The present embodiment yield is 89.6%, purity 99.7%.
Embodiment 4
A kind of preparation method of the high-purity Sulpiride of environmental protection, includes the following steps：
It is prepared by S1, crude product
12g 2- methoxyl group -5- sulfamoylbenzoic acids methyl esters, -2 aminomethyl tetrahydro pyrrolidine of 6g N- ethyls are sent into anti-
It answers in container, 120g glycerine is added, stirs 26min in 92 DEG C of reaction 3h of temperature, addition 320g water under nitrogen protection, is cooled to room
Temperature, stopping are passed through nitrogen, continue to be cooled to 1 DEG C, stand 16min, filter, dry, obtain crude product；
S2, bamboo charcoal activation
10g bamboo powders are fermented 15 days using 1-2g EM bacterium solutions, dry, pulverize, immerse a concentration of 1.3mol/L sodium hydroxides
22h is stood in solution, is filtered, it is dry, it is sent into vacuum tank in 820 DEG C of heat preservation 32min of temperature, is dropped with the speed of 0.6 DEG C/min
It warms to room temperature, washs to being in neutrality, dry, pulverize, obtain Activated Bamboo；
S3, purifying crude
125g absolute ethyl alcohols are added into 16g crude products, in 92 DEG C of reflux 12min of temperature, is cooled to 1 DEG C, filters, be added
A concentration of 84wt% ethanol solutions of 120g are added 2.6g Activated Bamboos and continue the 14min that flows back, surpass in 92 DEG C of reflux 3min of temperature
Sonication 31min, supersonic frequency 22KHz, filtering, crystallization, vacuum drying, drying temperature are 56 DEG C, and vacuum degree is
0.042MPa obtains the high-purity Sulpiride of environmental protection；The present embodiment yield is 89.9%, purity 99.9%.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of the high-purity Sulpiride of environmental protection, which is characterized in that include the following steps：
It is prepared by S1, crude product
2- methoxyl group -5- sulfamoylbenzoic acids methyl esters, -2 aminomethyl tetrahydro pyrrolidine of N- ethyls are sent into reaction vessel, added
Enter glycerine, in 90-95 DEG C of reaction of temperature under nitrogen protection, water is added to stir, be cooled to room temperature, stopping is passed through nitrogen, continues to cool down
It to 0-2 DEG C, stands, filters, it is dry, obtain crude product；
S2, bamboo charcoal activation
Bamboo powder is fermented using EM bacterium solutions, dry, pulverize, immerse in sodium hydroxide solution and stand, filter, it is dry, it is sent into vacuum
Case high temperature activates, and washs to being in neutrality, dry, pulverize, obtain Activated Bamboo；
S3, purifying crude
Absolute ethyl alcohol is added into crude product, in 80-100 DEG C of reflux of temperature, is cooled to 0-2 DEG C, a concentration of 80- is added in filtering
95wt% ethanol solutions are added Activated Bamboo and continue to flow back, be ultrasonically treated in 80-100 DEG C of reflux of temperature, filtering, crystallization, very
Sky is dry, obtains the high-purity Sulpiride of environmental protection.
2. the preparation method of the high-purity Sulpiride of environmental protection according to claim 1, which is characterized in that in S1,2- methoxyl groups-
The weight ratio 2-4 of 5- sulfamoylbenzoic acids methyl esters, -2 aminomethyl tetrahydro pyrrolidine of N- ethyls：1-2.
3. the preparation method of the high-purity Sulpiride of environmental protection according to claim 1, which is characterized in that in S1, nitrogen protection
Under in the reaction of 90-95 DEG C of temperature, reaction time 2-4h.
4. the preparation method of the high-purity Sulpiride of environmental protection according to claim 1, which is characterized in that in S2, bamboo powder and EM
The weight ratio of bacterium solution is 10：The pH value 3.5-4.5 of 1-2, EM bacterium solution.
5. the preparation method of the high-purity Sulpiride of environmental protection according to claim 1, which is characterized in that in S2, be sent into vacuum
Case high temperature activates, and first in 800-840 DEG C of heat preservation 20-40min of temperature, is then cooled to the speed of 0.2-0.8 DEG C/min
Room temperature.
6. the preparation method of the high-purity Sulpiride of environmental protection according to claim 1, which is characterized in that in S3, by weight
100-200 parts of absolute ethyl alcohols are added into 10-20 parts of crude products, in 80-100 DEG C of reflux 5-15min of temperature, are cooled to 0-2 DEG C, mistake
100-140 parts of a concentration of 80-95wt% ethanol solutions are added in filter, in 80-100 DEG C of reflux 2-5min of temperature.
7. the preparation method of the high-purity Sulpiride of environmental protection according to claim 1, which is characterized in that in S3, crude product, activation
The weight ratio of bamboo charcoal is 5-10：1-2.
8. the preparation method of the high-purity Sulpiride of environmental protection according to claim 1, which is characterized in that in S3, activation is added
Bamboo charcoal continues the 10-20min that flows back, and is ultrasonically treated 10-40min, supersonic frequency 20-30KHz.
9. the preparation method of the high-purity Sulpiride of environmental protection according to claim 1, which is characterized in that in S3, vacuum drying
In the process, drying temperature is 50-60 DEG C, vacuum degree 0.01-0.05MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112441960A (en) * | 2020-12-14 | 2021-03-05 | 常州康普药业有限公司 | Synthetic method of sulpiride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112441960A (en) * | 2020-12-14 | 2021-03-05 | 常州康普药业有限公司 | Synthetic method of sulpiride |
| CN112441960B (en) * | 2020-12-14 | 2022-03-01 | 常州康普药业有限公司 | Synthetic method of sulpiride |
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Application publication date: 20180731 |