CN107245063A - A kind of chlorpromazine training department and its preparation technology - Google Patents
A kind of chlorpromazine training department and its preparation technology Download PDFInfo
- Publication number
- CN107245063A CN107245063A CN201710581398.6A CN201710581398A CN107245063A CN 107245063 A CN107245063 A CN 107245063A CN 201710581398 A CN201710581398 A CN 201710581398A CN 107245063 A CN107245063 A CN 107245063A
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- China
- Prior art keywords
- chlorpromazine
- petroleum ether
- chloro
- training department
- water
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D279/00—Heterocyclic compounds containing six-membered rings having one nitrogen atom and one sulfur atom as the only ring hetero atoms
- C07D279/10—1,4-Thiazines; Hydrogenated 1,4-thiazines
- C07D279/14—1,4-Thiazines; Hydrogenated 1,4-thiazines condensed with carbocyclic rings or ring systems
- C07D279/18—[b, e]-condensed with two six-membered rings
- C07D279/22—[b, e]-condensed with two six-membered rings with carbon atoms directly attached to the ring nitrogen atom
- C07D279/24—[b, e]-condensed with two six-membered rings with carbon atoms directly attached to the ring nitrogen atom with hydrocarbon radicals, substituted by amino radicals, attached to the ring nitrogen atom
- C07D279/28—[b, e]-condensed with two six-membered rings with carbon atoms directly attached to the ring nitrogen atom with hydrocarbon radicals, substituted by amino radicals, attached to the ring nitrogen atom with other substituents attached to the ring system
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of chlorpromazine training department and its preparation technology, it is made up of 2 chloro phenothiazines, the methylaminopropane of 1 chlorine 3, solid NaOH, toluene, water, hydrochloric acid, activated carbon and petroleum ether, technical scheme disclosed in this invention can effectively improve chlorpromazine training department yield, required practical prices of raw materials relative moderate, and duration used in whole production technology is shorter, material cost negative demand amount to enterprise is small, possesses higher economic value.
Description
Technical field
The present invention relates to fine chemicals preparing technical field, specially a kind of chlorpromazine training department and its preparation technology.
Background technology
This noun of fine chemicals, is in use for a long time, and original refers to that yield is small, purity is high, price chemical products, such as cures
Medicine, dyestuff, coating etc..But, this implication is also without the essence for fully disclosing fine chemicals.Various countries expert is to essence in recent years
The definition of thin chemicals has some new opinions, it is American-European some it is national yield it is small, produced by different chemical structures and
The chemical substance of sale, referred to as fine chemicals (fine chemicals)；Yield it is small, by processing prepare, with special
The product of function or end-use properties, referred to as specialty chemicals.China, Japan etc. then are referred to as this two classes product to become more meticulous
Product.
Chlorpromazine training department be it is a kind of apply wider fine chemicals, chlorpromazine training department be mainly used in organic synthesis, medicine,
The intermediate of pesticide synthesis.The chemicals in industrial processes its purity, to prepare speed be limit its yield main
Factor.
The content of the invention
Chlorpromazine training department yield, the required practical prices of raw materials are effectively improved it is an object of the invention to provide one kind
Relative moderate, and duration used in whole production technology is shorter, and the material cost negative demand amount to enterprise is small, possesses higher warp
Ji value, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides following technical scheme：A kind of chlorpromazine training department, by 2- chloro phenothiazines, 1-
Chloro- 3- methylaminopropanes, solid NaOH, toluene, water, hydrochloric acid, activated carbon and petroleum ether according to following weight percents composition
Composition：
2- chloro phenothiazines 12 ~ 14%；
The chloro- 3- methylaminopropanes 14 ~ 16% of 1-；
Solid NaOH 9 ~ 10%；
Toluene 18 ~ 19%；
Water 13 ~ 15%；
Hydrochloric acid 11 ~ 12%；
Activated carbon 0.2%；
Petroleum ether 18 ~ 19%.
It is preferred that, a kind of chlorpromazine training department, by 2- chloro phenothiazines, the chloro- 3- methylaminopropanes of 1-, solid NaOH, toluene,
Water, hydrochloric acid, activated carbon and petroleum ether are constituted according to the composition of following weight percents：
2- chloro phenothiazines 13%；
The chloro- 3- methylaminopropanes 14.9% of 1-；
Solid NaOH 9.3%；
Toluene 18.6%；
Water 13.9%；
Hydrochloric acid 11.6%；
Activated carbon 0.2%；
Petroleum ether 18.5%.
The preparation technology of such a chlorpromazine training department, comprises the following steps：
（1）2- chloro phenothiazines, solid NaOH, toluene are added into condensation kettle, 100~120 DEG C of temperature is controlled, the chloro- 3- of 1- are added dropwise
Methylaminopropane carries out back flow reaction, and maintains the reflux for band water 6 hours；
（2）Reaction solution is cooled down, plus 70 DEG C of unreacted solid caustic soda of hot water dissolving, static layering, point sub-cloud aqueous phase, alkali waste water warp
Discharged after processing is qualified;
（3）By material be pumped into acidifying pot, be dissolved in water, control 70~75 DEG C of temperature, into kettle be added dropwise hydrochloric acid be acidified to pH value 2~
3 be terminal, static, and lower floor's spent acid moisture is gone, and activated carbon decolorizing is added in backward feed liquid, through nitrogen press filtration, removes useless live
Property charcoal, filtrate reclaims toluene after vacuum distillation, obtains crude product chlorpromazine training department；
（4）By step（3）Middle resulting material is cooled to 35~40 DEG C, adds petroleum ether, is removed by solvent of petroleum ether organic miscellaneous
Matter, and continue material being cooled to 0~3 DEG C, chlorpromazine training department crystallizes in petroleum ether；
（5）Crystal solution is centrifuged, filtrate is petroleum ether and organic impurities mixture, and petroleum ether is reclaimed through soda acidization,
For applying mechanically, three-protection design is periodically carried out, filter cake is the chlorpromazine training department after refining.
It is preferred that, step（3）Middle distillation pressure is -0.09Mpa, and vapo(u)rizing temperature is 120~140 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：
Technical scheme disclosed in this invention can effectively improve chlorpromazine training department yield, and the required practical prices of raw materials are relative
It is cheap, and duration used in whole production technology is shorter, and the material cost negative demand amount to enterprise is small, possesses higher economic valency
Value.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
Embodiment 1
The present invention provides a kind of technical scheme：A kind of chlorpromazine training department, by 2- chloro phenothiazines, the chloro- 3- methylaminopropanes of 1-, solid
NaOH, toluene, water, hydrochloric acid, activated carbon and petroleum ether are constituted according to the composition of following weight percents：
2- chloro phenothiazines 12 ~ 14%；
The chloro- 3- methylaminopropanes 14 ~ 16% of 1-；
Solid NaOH 9 ~ 10%；
Toluene 18 ~ 19%；
Water 13 ~ 15%；
Hydrochloric acid 11 ~ 12%；
Activated carbon 0.2%；
Petroleum ether 18 ~ 19%.
The preparation technology of such a chlorpromazine training department, comprises the following steps：
（1）2- chloro phenothiazines, solid NaOH, toluene are added into condensation kettle, 100~120 DEG C of temperature is controlled, the chloro- 3- of 1- are added dropwise
Methylaminopropane carries out back flow reaction, and maintains the reflux for band water 6 hours；
（2）Reaction solution is cooled down, plus 70 DEG C of unreacted solid caustic soda of hot water dissolving, static layering, point sub-cloud aqueous phase, alkali waste water warp
Discharged after processing is qualified;
（3）By material be pumped into acidifying pot, be dissolved in water, control 70~75 DEG C of temperature, into kettle be added dropwise hydrochloric acid be acidified to pH value 2~
3 be terminal, static, and lower floor's spent acid moisture is gone, and activated carbon decolorizing is added in backward feed liquid, through nitrogen press filtration, removes useless live
Property charcoal, filtrate reclaims toluene after vacuum distillation, obtains crude product chlorpromazine training department, step（3）Middle distillation pressure is -0.09Mpa, is steamed
Temperature is evaporated for 120~140 DEG C.
（4）By step（3）Middle resulting material is cooled to 35~40 DEG C, adds petroleum ether, being removed by solvent of petroleum ether has
Machine impurity, and continue material being cooled to 0~3 DEG C, chlorpromazine training department crystallizes in petroleum ether；
（5）Crystal solution is centrifuged, filtrate is petroleum ether and organic impurities mixture, and petroleum ether is reclaimed through soda acidization,
For applying mechanically, three-protection design is periodically carried out, filter cake is the chlorpromazine training department after refining.
Technical scheme disclosed in this invention can effectively improve chlorpromazine training department yield, the required practical prices of raw materials
Relative moderate, and duration used in whole production technology is shorter, and the material cost negative demand amount to enterprise is small, possesses higher warp
Ji value.
Embodiment 2
A kind of chlorpromazine training department, by 2- chloro phenothiazines, the chloro- 3- methylaminopropanes of 1-, solid NaOH, toluene, water, hydrochloric acid, activity
Charcoal and petroleum ether are constituted according to the composition of following weight percents：
2- chloro phenothiazines 13%；
The chloro- 3- methylaminopropanes 14.9% of 1-；
Solid NaOH 9.3%；
Toluene 18.6%；
Water 13.9%；
Hydrochloric acid 11.6%；
Activated carbon 0.2%；
Petroleum ether 18.5%.
The preparation technology of such a chlorpromazine training department, comprises the following steps：
（1）2- chloro phenothiazines, solid NaOH, toluene are added into condensation kettle, 100~120 DEG C of temperature is controlled, the chloro- 3- of 1- are added dropwise
Methylaminopropane carries out back flow reaction, and maintains the reflux for band water 6 hours；
（2）Reaction solution is cooled down, plus 70 DEG C of unreacted solid caustic soda of hot water dissolving, static layering, point sub-cloud aqueous phase, alkali waste water warp
Discharged after processing is qualified;
（3）By material be pumped into acidifying pot, be dissolved in water, control 70~75 DEG C of temperature, into kettle be added dropwise hydrochloric acid be acidified to pH value 2~
3 be terminal, static, and lower floor's spent acid moisture is gone, and activated carbon decolorizing is added in backward feed liquid, through nitrogen press filtration, removes useless live
Property charcoal, filtrate reclaims toluene after vacuum distillation, obtains crude product chlorpromazine training department, step（3）Middle distillation pressure is -0.09Mpa, is steamed
Temperature is evaporated for 120~140 DEG C.
（4）By step（3）Middle resulting material is cooled to 35~40 DEG C, adds petroleum ether, being removed by solvent of petroleum ether has
Machine impurity, and continue material being cooled to 0~3 DEG C, chlorpromazine training department crystallizes in petroleum ether；
（5）Crystal solution is centrifuged, filtrate is petroleum ether and organic impurities mixture, and petroleum ether is reclaimed through soda acidization,
For applying mechanically, three-protection design is periodically carried out, filter cake is the chlorpromazine training department after refining.
Technical scheme disclosed in this invention can effectively improve chlorpromazine training department yield, the required practical prices of raw materials
Relative moderate, and duration used in whole production technology is shorter, and the material cost negative demand amount to enterprise is small, possesses higher warp
Ji value.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (4)
1. a kind of chlorpromazine training department, it is characterised in that：By 2- chloro phenothiazines, the chloro- 3- methylaminopropanes of 1-, solid NaOH, toluene,
Water, hydrochloric acid, activated carbon and petroleum ether are constituted according to the composition of following weight percents：
2- chloro phenothiazines 12 ~ 14%；
The chloro- 3- methylaminopropanes 14 ~ 16% of 1-；
Solid NaOH 9 ~ 10%；
Toluene 18 ~ 19%；
Water 13 ~ 15%；
Hydrochloric acid 11 ~ 12%；
Activated carbon 0.2%；
Petroleum ether 18 ~ 19%.
2. a kind of chlorpromazine training department according to claim 1, it is characterised in that：By 2- chloro phenothiazines, the chloro- 3- methylaminos of 1-
Propane, solid NaOH, toluene, water, hydrochloric acid, activated carbon and petroleum ether are constituted according to the composition of following weight percents：
2- chloro phenothiazines 13%；
The chloro- 3- methylaminopropanes 14.9% of 1-；
Solid NaOH 9.3%；
Toluene 18.6%；
Water 13.9%；
Hydrochloric acid 11.6%；
Activated carbon 0.2%；
Petroleum ether 18.5%.
3. realize a kind of preparation technology of chlorpromazine training department described in claim 1, it is characterised in that：Comprise the following steps：
（1）2- chloro phenothiazines, solid NaOH, toluene are added into condensation kettle, 100~120 DEG C of temperature is controlled, the chloro- 3- of 1- are added dropwise
Methylaminopropane carries out back flow reaction, and maintains the reflux for band water 6 hours；
（2）Reaction solution is cooled down, plus 70 DEG C of unreacted solid caustic soda of hot water dissolving, static layering, point sub-cloud aqueous phase, alkali waste water warp
Discharged after processing is qualified;
（3）By material be pumped into acidifying pot, be dissolved in water, control 70~75 DEG C of temperature, into kettle be added dropwise hydrochloric acid be acidified to pH value 2~
3 be terminal, static, and lower floor's spent acid moisture is gone, and activated carbon decolorizing is added in backward feed liquid, through nitrogen press filtration, removes useless live
Property charcoal, filtrate reclaims toluene after vacuum distillation, obtains crude product chlorpromazine training department；
（4）By step（3）Middle resulting material is cooled to 35~40 DEG C, adds petroleum ether, is removed by solvent of petroleum ether organic miscellaneous
Matter, and continue material being cooled to 0~3 DEG C, chlorpromazine training department crystallizes in petroleum ether；
（5）Crystal solution is centrifuged, filtrate is petroleum ether and organic impurities mixture, and petroleum ether is reclaimed through soda acidization,
For applying mechanically, three-protection design is periodically carried out, filter cake is the chlorpromazine training department after refining.
4. a kind of preparation technology of chlorpromazine training department according to claim 3, it is characterised in that：The step（3）It is middle to steam
Pressure is evaporated for -0.09Mpa, and vapo(u)rizing temperature is 120~140 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710581398.6A CN107245063A (en) | 2017-07-17 | 2017-07-17 | A kind of chlorpromazine training department and its preparation technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710581398.6A CN107245063A (en) | 2017-07-17 | 2017-07-17 | A kind of chlorpromazine training department and its preparation technology |
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| Publication Number | Publication Date |
|---|---|
| CN107245063A true CN107245063A (en) | 2017-10-13 |
Family
ID=60014553
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710581398.6A Pending CN107245063A (en) | 2017-07-17 | 2017-07-17 | A kind of chlorpromazine training department and its preparation technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3533790A3 (en) * | 2018-03-03 | 2019-09-25 | Solara Active Pharma Sciences Limited | An improved process for preparation of chlorpromazine or its pharmaceutically acceptable salts |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617509A (en) * | 2012-03-15 | 2012-08-01 | 常州康普药业有限公司 | Chlorpromazine hydrochloride synthesis process |
-
2017
- 2017-07-17 CN CN201710581398.6A patent/CN107245063A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617509A (en) * | 2012-03-15 | 2012-08-01 | 常州康普药业有限公司 | Chlorpromazine hydrochloride synthesis process |
Non-Patent Citations (1)
| Title |
|---|
| LAMECK F S CHAGONDA ET AL.,: "The determination of chlorpromazine, related impurities and degradation products in pharmaceutical dosage forms", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3533790A3 (en) * | 2018-03-03 | 2019-09-25 | Solara Active Pharma Sciences Limited | An improved process for preparation of chlorpromazine or its pharmaceutically acceptable salts |
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Application publication date: 20171013 |