CN109942412A - The recyclable device of aceticanhydride in a kind of 5- bromo indole preparation process - Google Patents
The recyclable device of aceticanhydride in a kind of 5- bromo indole preparation process Download PDFInfo
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- CN109942412A CN109942412A CN201910270153.0A CN201910270153A CN109942412A CN 109942412 A CN109942412 A CN 109942412A CN 201910270153 A CN201910270153 A CN 201910270153A CN 109942412 A CN109942412 A CN 109942412A
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- aceticanhydride
- flowmeter
- rectifying column
- preparation process
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Abstract
The recyclable device of aceticanhydride in one 5- bromo indole preparation process of disclosure of the invention, including distillation still, rectifying column, condenser, water segregator, first flowmeter and second flowmeter；The rectifying column is set to the top of distillation still, is connected with distillation still；Outlet at the top of the rectifying column is connected by the material inlet of conveyance conduit and condenser；The material outlet of condenser is connected by one end of condensation branch pipe and first flowmeter and general pipeline；The other end of the general pipeline and the entrance of water segregator connect；The general pipeline also passes through second flowmeter and water pipe and connect with water service device；Toluene outlet at the top of the water segregator is connected by the toluene recovery mouth of refluxing toluene pipeline and rectifying column, and the present invention efficiently separates aceticanhydride and acetic acid.
Description
Technical field
The invention belongs to field of medicine and chemical technology, and in particular to the recyclable device of aceticanhydride in a kind of 5- bromo indole preparation process.
Background technique
5- bromo indole is that one kind is used in the drugs such as prevention and cure of cardiovascular disease, neurological disease, tumour and strengthen immunity
Very extensive intermediate, important use first is that secondary colour aminated compounds, wherein epiphysin and its derivative are given birth to adjusting
It manages rhythm and sleep, anti-tumor aspect is largely effective.5- methoxyl group -2- phenyl tryptamines has antitumaous effect.Serotonine exists
Control smoking addiction in terms of play the role of it is special, cardiovascular disease and mental disease prevention and treatment and it is anti-in terms of also have it is bright
Aobvious effect.
5- bromo indole is that the first step is reacted with sodium hydrogensulfite generates 2- sodium sulfonate indoline using indoles as starting material,
Second step is reacted with aceticanhydride generates N- acetyl group -2- sodium sulfonate indoline, and third step reacts preparation 5- bromo indole with bromine.
5- bromo indole needs to be excessively used during the preparation process aceticanhydride, and acylation reaction generates acetic acid simultaneously, due in aceticanhydride
Containing acetic acid, it is unable to direct circulation and applies.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of recyclable devices of aceticanhydride in 5- bromo indole preparation process, by vinegar
Acid anhydride and separated from acetic acid.
In order to solve the above technical problems, the present invention adopts the following technical scheme that: aceticanhydride in a kind of 5- bromo indole preparation process
Recyclable device, including distillation still, rectifying column, condenser, water segregator, first flowmeter and second flowmeter；The rectifying
Tower is set to the top of distillation still, is connected with distillation still；Outlet at the top of the rectifying column passes through conveyance conduit and condenser
Material inlet connection；The material outlet of condenser is connected by one end of condensation branch pipe and first flowmeter and general pipeline；Described
The other end of general pipeline and the entrance of water segregator connect；The general pipeline also passes through second flowmeter and water pipe and water service fills
Set connection；Toluene outlet at the top of the water segregator is connected by the toluene recovery mouth of refluxing toluene pipeline and rectifying column.
Further, heating device is provided with outside the distillation still.
Further, the pipeline bottom is provided with acetic acid aqueous solution outlet, the acetic acid aqueous solution exit
It is provided with switch valve.
Further, switch valve is provided on the water pipe and the condensation branch pipe.
Beneficial effects of the present invention: by used aceticanhydride in 5- bromo indole preparation process, by the way that toluene distillation is added, point
Acetic acid is separated out, water segregator removal acetic acid is added water, obtains the aceticanhydride that can be recycled, structure and simple process.
Detailed description of the invention
It, below will be to needed in the embodiment in order to more clearly illustrate the technical solution in the embodiment of the present invention
Attached drawing is simply introduced, it should be apparent that, the accompanying drawings in the following description is only some embodiments recorded in the present invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is the structural diagram of the present invention.
Specific embodiment
Technical solution of the present invention will be clearly and completely described by specific embodiment below.
As shown in Figure 1, for the recyclable device of aceticanhydride in a kind of 5- bromo indole preparation process of the invention, including distillation still 1,
Rectifying column 2, condenser 3, water segregator 4, first flowmeter 5 and second flowmeter 6；The rectifying column 2 is set to distillation still 1
Top is connected with distillation still 1；The outlet at 2 top of rectifying column is connect by conveyance conduit 7 with the material inlet of condenser 3；
The material outlet of condenser 3 is connect by condensation branch pipe 8 and first flowmeter 5 with one end of general pipeline 9；The general pipeline's 9 is another
One end is connect with the entrance of water segregator 4；The general pipeline 9 also passes through second flowmeter 6 and water pipe 10 and water service device
11 connections；Water service device 11 can be tap or water tank etc..It is provided with out on water pipe 10 and condensation branch pipe 8
Close valve.The toluene outlet at 4 top of water segregator is connect by refluxing toluene pipeline 12 with the toluene recovery mouth of rectifying column 2.Point
4 bottom of hydrophone is provided with acetic acid aqueous solution outlet 13, is provided with switch valve at acetic acid aqueous solution outlet 13.
Heating device is provided with outside distillation still 1.Heating device is the prior art, and details are not described herein.The preparation of 5- bromo indole
Used aceticanhydride adds water water segregator removal acetic acid, obtains being recycled by the way that toluene distillation is added in the process
Aceticanhydride opens the valve of water pipe in distillation process, and adjusting second flowmeter flow is about the 25-30% for distilling out the amount of evaporating,
Acetic acid aqueous solution is separated in water segregator, upper toluene flows back into rectifying column.When pot temperature reaches 110 DEG C, stopping divides water,
Toluene is steamed, when pot temperature reaches 136 DEG C, stopping distillation being cooled to room temperature, obtains the aceticanhydride that can be recycled.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to design of the invention
It is defined with range, without departing from the design concept of the invention, ordinary engineering and technical personnel is to this hair in this field
The all variations and modifications that bright technical solution is made should all fall into protection scope of the present invention, claimed skill of the invention
Art content is all documented in technical requirements book.
Claims (4)
1. the recyclable device of aceticanhydride in a kind of 5- bromo indole preparation process, it is characterised in that: including distillation still (1), rectifying column
(2), condenser (3), water segregator (4), first flowmeter (5) and second flowmeter (6)；The rectifying column (2) is set to steaming
The top for evaporating kettle (1) is connected with distillation still (1)；Outlet at the top of the rectifying column (2) passes through conveyance conduit (7) and condenser
(3) material inlet connection；The material outlet of condenser (3) passes through condensation branch pipe (8) and first flowmeter (5) and general pipeline (9)
One end connection；The other end of the general pipeline (9) is connect with the entrance of water segregator (4)；The general pipeline (9) also passes through second
Flowmeter (6) and water pipe (10) are connect with water service device (11)；Toluene outlet at the top of the water segregator (4) passes through first
Benzene reflux line (12) is connect with the toluene recovery mouth of rectifying column (2).
2. the recyclable device of aceticanhydride in a kind of 5- bromo indole preparation process according to claim 1, it is characterised in that: described
Distillation still (1) outside be provided with heating device.
3. the recyclable device of aceticanhydride in a kind of 5- bromo indole preparation process according to claim 1, it is characterised in that: described
Water segregator (4) bottom be provided with acetic acid aqueous solution outlet (13), be provided with switch at the described acetic acid aqueous solution outlet (13)
Valve.
4. the recyclable device of aceticanhydride in a kind of 5- bromo indole preparation process according to claim 1, it is characterised in that: described
Water pipe (10) and the condensation branch pipe (8) on be provided with switch valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910270153.0A CN109942412A (en) | 2019-04-04 | 2019-04-04 | The recyclable device of aceticanhydride in a kind of 5- bromo indole preparation process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910270153.0A CN109942412A (en) | 2019-04-04 | 2019-04-04 | The recyclable device of aceticanhydride in a kind of 5- bromo indole preparation process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109942412A true CN109942412A (en) | 2019-06-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910270153.0A Pending CN109942412A (en) | 2019-04-04 | 2019-04-04 | The recyclable device of aceticanhydride in a kind of 5- bromo indole preparation process |
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| Country | Link |
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| CN (1) | CN109942412A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000302725A (en) * | 1999-04-21 | 2000-10-31 | Daicel Chem Ind Ltd | Distillation purifying equipment for acetic anhydride |
| CN102558017A (en) * | 2011-12-27 | 2012-07-11 | 郑州凯美克化学有限公司 | Method for preparing 5-bromoindole |
| CN105175261A (en) * | 2015-09-22 | 2015-12-23 | 山东新和成药业有限公司 | Method for performing acetylation by means of acetic anhydride |
| CN208065817U (en) * | 2018-02-11 | 2018-11-09 | 宁波王龙科技股份有限公司 | A kind of novel aceticanhydride rectifying vacuum system |
-
2019
- 2019-04-04 CN CN201910270153.0A patent/CN109942412A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000302725A (en) * | 1999-04-21 | 2000-10-31 | Daicel Chem Ind Ltd | Distillation purifying equipment for acetic anhydride |
| CN102558017A (en) * | 2011-12-27 | 2012-07-11 | 郑州凯美克化学有限公司 | Method for preparing 5-bromoindole |
| CN105175261A (en) * | 2015-09-22 | 2015-12-23 | 山东新和成药业有限公司 | Method for performing acetylation by means of acetic anhydride |
| CN208065817U (en) * | 2018-02-11 | 2018-11-09 | 宁波王龙科技股份有限公司 | A kind of novel aceticanhydride rectifying vacuum system |
Non-Patent Citations (2)
| Title |
|---|
| 刘平: "吲哚5位和3位取代化合物的合成研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 张敏，袁先友 著: "《杂多酸催化精细有机合成反应研究》", 31 October 2008, 吉林大学出版社 * |
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Application publication date: 20190628 |