CN211358769U - Synthesis device of S-4-chloro-3-hydroxybutyric acid ethyl ester - Google Patents
Synthesis device of S-4-chloro-3-hydroxybutyric acid ethyl ester Download PDFInfo
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- CN211358769U CN211358769U CN201921693681.9U CN201921693681U CN211358769U CN 211358769 U CN211358769 U CN 211358769U CN 201921693681 U CN201921693681 U CN 201921693681U CN 211358769 U CN211358769 U CN 211358769U
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- ethyl
- chloro
- ethyl butyrate
- condenser
- synthesis kettle
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- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 51
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 50
- OBNCKNCVKJNDBV-UHFFFAOYSA-N butanoic acid ethyl ester Natural products CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 claims abstract description 49
- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000010521 absorption reaction Methods 0.000 claims abstract description 18
- 239000003513 alkali Substances 0.000 claims abstract description 18
- DZGCGKFAPXFTNM-UHFFFAOYSA-N ethanol;hydron;chloride Chemical compound Cl.CCO DZGCGKFAPXFTNM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000010992 reflux Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000009833 condensation Methods 0.000 claims description 16
- 230000005494 condensation Effects 0.000 claims description 16
- 230000002194 synthesizing effect Effects 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- ZAJNMXDBJKCCAT-YFKPBYRVSA-N ethyl (3s)-4-chloro-3-hydroxybutanoate Chemical compound CCOC(=O)C[C@H](O)CCl ZAJNMXDBJKCCAT-YFKPBYRVSA-N 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 6
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OJRHUICOVVSGSY-RXMQYKEDSA-N (2s)-2-chloro-3-methylbutan-1-ol Chemical compound CC(C)[C@H](Cl)CO OJRHUICOVVSGSY-RXMQYKEDSA-N 0.000 description 1
- 238000003482 Pinner synthesis reaction Methods 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 229960001770 atorvastatin calcium Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229960000672 rosuvastatin Drugs 0.000 description 1
- BPRHUIZQVSMCRT-VEUZHWNKSA-N rosuvastatin Chemical compound CC(C)C1=NC(N(C)S(C)(=O)=O)=NC(C=2C=CC(F)=CC=2)=C1\C=C\[C@@H](O)C[C@@H](O)CC(O)=O BPRHUIZQVSMCRT-VEUZHWNKSA-N 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a synthesizer of S-4-chlorine-3-hydroxybutyric acid ethyl ester, including the synthetic cauldron of ethyl butyrate, synthesizer still includes: the hydrochloric acid ethanol storage tank is communicated with the ethyl butyrate synthesis kettle through a feeding pipe; the S-4-chloro-3-hydroxybutyronitrile storage tank is communicated with the ethyl butyrate synthesis kettle through a feeding pipe; the jacket is sleeved outside the ethyl butyrate synthesis kettle and used for controlling the reaction temperature in the ethyl butyrate synthesis kettle; the inlet and the outlet of the condenser are both communicated with the ethyl butyrate synthesis kettle; a tail gas absorption tank connected to an outlet of the condenser; wherein, the tail gas absorption tank is stored with alkali solution. Accurately controlling the temperature of the reflux reaction in the kettle, and optimizing production; through the setting of alkali lye in the tail gas absorption tank, can absorb the acid tail gas that the reaction back discharged completely, the pollution abatement is more environmental protection.
Description
Technical Field
The utility model relates to a chemical synthesis equipment technical field, more specifically relates to a synthesizer of S-4-chlorine-3-hydroxybutyric acid ethyl ester.
Background
The S-4-chloro-3-hydroxy ethyl butyrate is a chiral drug intermediate with wide application, and can be used for synthesizing atorvastatin calcium, rosuvastatin and other drugs.
The method is characterized in that ethanol hydrochloride and S-4-chloro-3-hydroxybutyronitrile are used as raw materials and undergo a Pinner reaction to prepare the ethyl S-4-chloro-3-hydroxybutyrate, however, in the process of preparing the ethyl S-4-chloro-3-hydroxybutyrate, the ethanol hydrochloride is easy to boil under the temperature condition required by the reaction due to low boiling point and extremely easy volatilization, and if a reaction kettle is directly communicated with a tail gas treatment device, the ethanol hydrochloride is seriously volatilized and lost at the reaction temperature, so that the reaction effect cannot be ensured; if the reaction kettle is closed, the pressure of the reaction kettle can be greatly increased after the hydrochloric acid ethanol is boiled and volatilized, and danger is easy to occur.
Therefore, it is necessary to develop a synthesis apparatus for ethyl S-4-chloro-3-hydroxybutyrate, which not only can ensure the reaction effect, but also can solve the problem of volatilization loss of the raw material ethanol hydrochloride, and is beneficial to environmental protection and improvement of the working environment of workers by considering the treatment of waste gas.
The information disclosed in this background section of the invention is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information constitutes prior art already known to a person skilled in the art.
SUMMERY OF THE UTILITY MODEL
To the problem that prior art exists, the utility model provides a synthesizer of S-4-chlorine-3-hydroxyl ethyl butyrate, the reflux reaction that can accurate control ethyl butyrate through synthesizer' S structural design, accurate control reflux reaction temperature absorbs the tail gas after the reaction, has realized the dual purpose of optimized production and environmental protection.
In order to achieve the above purpose, the utility model adopts the following technical scheme: the synthesis device of the S-4-chloro-3-hydroxybutanoic acid ethyl ester comprises an ethyl butyrate synthesis kettle, and further comprises:
the hydrochloric acid ethanol storage tank is communicated with the ethyl butyrate synthesis kettle through a feeding pipe;
the S-4-chloro-3-hydroxybutyronitrile storage tank is communicated with the ethyl butyrate synthesis kettle through a feeding pipe;
the jacket is sleeved outside the ethyl butyrate synthesis kettle and used for controlling the reaction temperature in the ethyl butyrate synthesis kettle;
the inlet and the outlet of the condenser are both communicated with the ethyl butyrate synthesis kettle;
a tail gas absorption tank connected to an outlet of the condenser;
wherein, the tail gas absorption tank is stored with alkali solution.
Preferably, the synthesis apparatus further comprises:
and the stirring paddle is arranged in the ethyl butyrate synthesis kettle and is used for stirring reactants in the ethyl butyrate synthesis kettle.
Preferably, the inlet of the condenser is communicated with the ethyl butyrate synthesis kettle through an air duct, and the outlet of the condenser is communicated with the ethyl butyrate synthesis kettle through a condensing pipe.
Preferably, the tail gas absorption tank is communicated with the condensation pipe through a tail gas pipe.
Preferably, a water flushing pump is arranged on the tail gas pipe and used for giving reaction micro negative pressure.
Preferably, a sight glass is arranged on the condensation pipe and used for monitoring the condensation reflux state.
Preferably, a switch valve is arranged on the condensation pipe and used for controlling the reflux of the condenser.
Preferably, the feed pipe is provided with a switch valve for controlling the feeding amount.
Preferably, a steam pipe, a steam condensation pipe, a circulating water inlet pipe and a circulating water outlet pipe are respectively connected outside the jacket.
Preferably, the alkali solution is 28% -35% alkali solution.
The utility model has the advantages that: a steam pipe, a steam condensation pipe, a circulating water inlet pipe and a circulating water outlet pipe are arranged outside the jacket, so that the reflux reaction temperature in the kettle is accurately controlled, and the production is optimized; through the setting of alkali lye in the tail gas absorption tank, can absorb the acid tail gas that the reaction back discharged completely, the pollution abatement is more environmental protection.
The synthesis device of the invention has other features and advantages which will be apparent from or are set forth in detail in the accompanying drawings and the following detailed description, which are incorporated herein, and which together serve to explain certain principles of the invention.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments of the present invention with reference to the attached drawings, in which like reference numerals generally represent like parts in exemplary embodiments of the present invention.
Fig. 1 shows a schematic diagram of a synthesis apparatus of ethyl S-4-chloro-3-hydroxybutyrate according to an exemplary embodiment of the present invention.
Description of reference numerals:
1. a hydrochloric acid ethanol storage tank; 2. an S-4-chloro-3-hydroxybutyronitrile storage tank; 3. ethyl butyrate synthesizing kettle; 4. a condenser; 401. a low temperature water inlet pipe; 402. a low-temperature water outlet pipe; 403. a sight glass; 5. a tail gas absorption tank; 501. a water flush pump; 6. an on-off valve; 7. a jacket; 701. a steam pipe; 702. a steam condenser pipe; 703. a circulating water inlet pipe; 704. a circulating water outlet pipe; 8. and (4) a stirring paddle.
Detailed Description
The invention will be described in more detail below with reference to the accompanying drawings. While the preferred embodiments of the present invention have been illustrated in the accompanying drawings, it is to be understood that the invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Fig. 1 shows a schematic diagram of a synthesis apparatus of ethyl S-4-chloro-3-hydroxybutyrate according to an exemplary embodiment of the present invention. (in FIG. 1, the direction of the arrow indicates the direction of flow of water or gas)
As shown in fig. 1, the utility model provides a synthesizer of S-4-chlorine-3-hydroxy ethyl butyrate, including synthetic cauldron 3 of ethyl butyrate, synthesizer still includes:
the hydrochloric acid ethanol storage tank 1 is communicated with the ethyl butyrate synthesis kettle 3 through a feeding pipe;
the S-4-chloro-3-hydroxybutyronitrile storage tank 2 is communicated with the ethyl butyrate synthesis kettle 3 through a feeding pipe;
the jacket 7 is sleeved outside the ethyl butyrate synthesis kettle 3, and is used for controlling the reaction temperature in the ethyl butyrate synthesis kettle 3;
the inlet and the outlet of the condenser 4 are communicated with the ethyl butyrate synthesis kettle 3;
a tail gas absorption tank 5 connected to an outlet of the condenser 4;
wherein, the tail gas absorption tank 5 is stored with alkali solution.
Further, the alkali solution is 28% -35% alkali solution, and preferably 30% alkali solution.
Because the concentration of the alkali liquor is too high, higher danger is generated, and if the alkali is completely reacted with the hydrogen chloride gas, the generated sodium chloride salt is easy to separate out, the treatment difficulty of the subsequent part is increased, and the concentration of the alkali liquor is too low, and the alkali liquor must be frequently replaced to achieve a better absorption effect, and the economy is not high, so that 30% alkali liquor is the optimal choice through repeated verification.
Preferably, the synthesizing apparatus further comprises:
and the stirring paddle 8 is arranged in the ethyl butyrate synthesis kettle 3 and is used for stirring reactants in the ethyl butyrate synthesis kettle 3.
The arrangement of the stirring paddle 8 enables the ethanol hydrochloride and the S-4-chloro-3-hydroxybutyronitrile entering the ethyl butyrate synthesis kettle 3 to be quickly mixed, so that the reaction is more sufficient, and the material waste is reduced.
As the preferred scheme, the inlet of the condenser 4 is communicated with the ethyl butyrate synthesis kettle 3 through a gas guide pipe, and the outlet of the condenser 4 is communicated with the ethyl butyrate synthesis kettle 3 through a condensing pipe.
Specifically, hydrogen chloride gas and ethanol volatilized from the ethyl butyrate synthesis kettle 3 enter the condenser 4 through the gas guide tube to be condensed and refluxed; a condensing pipe is connected below the condenser 4 and used for refluxing the condensed hydrogen chloride and ethanol to the ethyl butyrate synthesis kettle 3.
Furthermore, a viewing mirror 403 is arranged on the condensation pipe for monitoring the condensation reflux state, and a switch valve 6 is further arranged on the condensation pipe for controlling the reflux of the condenser 4.
Wherein, the condenser 4 is also externally connected with a low-temperature water inlet pipe 401 and a low-temperature water outlet pipe 402.
Wherein the temperature range of the low-temperature water is 5-10 ℃.
The condenser 4 inner loop be low temperature water for the volatile hydrogen chloride gas of condensation and ethanol, sight glass 403 on the condenser pipe is the unloading sight glass, is used for observing whether the volatile gas begins the condensation, whether the condensate begins the backward flow, simultaneously, is equipped with ooff valve 6 on the condenser pipe, is used for controlling the backward flow of condensate.
As the preferred scheme, the tail gas absorption tank 5 is communicated with the condensation pipe through a tail gas pipe.
Wherein, a water flushing pump 501 is arranged on the tail gas pipe and is used for giving a micro negative pressure to the reaction.
Further, the water flushing pump 501 is used for giving a slight negative pressure to the reaction, wherein the alkali solution in the tail gas absorption tank 5 can absorb the hydrogen chloride tail gas after the reaction, thereby completing the absorption of the tail gas.
The acid tail gas discharged after reaction can be completely absorbed by the arrangement of the alkali liquor in the tail gas absorption tank 5, so that the pollution is reduced, and the environment is protected.
Preferably, the feed pipe is provided with a switch valve 6 for controlling the feed amount.
The switching valve 6 can effectively control the feeding amount of the hydrochloric acid ethanol and the S-4-chloro-3-hydroxybutyronitrile, and can avoid the waste of raw materials.
Preferably, the jacket 7 is externally connected with a steam pipe 701, a steam condensation pipe 702, a circulating water inlet pipe 703 and a circulating water outlet pipe 704 respectively.
The reaction temperature in the ethyl butyrate synthesis kettle 3 is controlled to be 60-65 ℃, when the temperature is lower, steam can be introduced for heating, and when the temperature is higher, circulating water can be introduced for cooling.
The arrangement of the steam pipe 701, the steam condensation pipe 702, the circulating water inlet pipe 703 and the circulating water outlet pipe 704 can effectively control the reaction temperature in the ethyl butyrate synthesis kettle 3.
A steam pipe 701, a steam condensation pipe 702, a circulating water inlet pipe 703 and a circulating water outlet pipe 704 are arranged outside the jacket 7, so that the reflux reaction temperature in the kettle is accurately controlled, and the production is optimized.
The present invention and the embodiments thereof have been described above, but the description is not limited thereto, and the embodiment shown in the drawings is only one of the embodiments of the present invention, and the actual structure is not limited thereto. In summary, those skilled in the art should understand that they should not be limited to the embodiments described above, and that they can design the similar structure and embodiments without departing from the spirit of the invention.
Claims (9)
1. The synthesis device of the S-4-chloro-3-hydroxy ethyl butyrate comprises an ethyl butyrate synthesis kettle, and is characterized by further comprising:
the hydrochloric acid ethanol storage tank is communicated with the ethyl butyrate synthesis kettle through a feeding pipe;
the S-4-chloro-3-hydroxybutyronitrile storage tank is communicated with the ethyl butyrate synthesis kettle through a feeding pipe;
the jacket is sleeved outside the ethyl butyrate synthesis kettle and used for controlling the reaction temperature in the ethyl butyrate synthesis kettle;
the inlet and the outlet of the condenser are both communicated with the ethyl butyrate synthesis kettle;
a tail gas absorption tank connected to an outlet of the condenser;
wherein, the tail gas absorption tank is stored with alkali solution.
2. The apparatus for synthesizing ethyl S-4-chloro-3-hydroxybutanoate according to claim 1, wherein said apparatus for synthesizing further comprises:
and the stirring paddle is arranged in the ethyl butyrate synthesis kettle and is used for stirring reactants in the ethyl butyrate synthesis kettle.
3. The synthesis device of ethyl-S-4-chloro-3-hydroxybutanoate as claimed in claim 1, wherein an inlet of the condenser is communicated with the ethyl-butanoate synthesis kettle through a gas-guide tube, and an outlet of the condenser is communicated with the ethyl-butanoate synthesis kettle through a condensation tube.
4. The apparatus for synthesizing ethyl S-4-chloro-3-hydroxybutanoate of claim 3, wherein the tail gas absorption tank is in communication with the condenser tube through a tail gas tube.
5. The apparatus for synthesizing ethyl S-4-chloro-3-hydroxybutyrate of claim 4, wherein the tail gas pipe is provided with a water flushing pump for giving a slight negative pressure to the reaction.
6. A synthesis unit of ethyl S-4-chloro-3-hydroxybutanoate, as recited in claim 3, wherein a view mirror is provided on the condenser tube for monitoring the condensate reflux condition.
7. The apparatus for synthesizing ethyl S-4-chloro-3-hydroxybutanoate according to claim 3, wherein a switch valve is provided on the condenser tube for controlling reflux of the condenser.
8. The apparatus for synthesizing ethyl S-4-chloro-3-hydroxybutanoate according to claim 1, wherein a switch valve is provided on the feed pipe for controlling the feed amount.
9. The apparatus for synthesizing ethyl S-4-chloro-3-hydroxybutanoate according to claim 1, wherein a steam pipe, a steam condenser pipe, a circulating water inlet pipe, and a circulating water outlet pipe are connected outside the jacket, respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921693681.9U CN211358769U (en) | 2019-10-11 | 2019-10-11 | Synthesis device of S-4-chloro-3-hydroxybutyric acid ethyl ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921693681.9U CN211358769U (en) | 2019-10-11 | 2019-10-11 | Synthesis device of S-4-chloro-3-hydroxybutyric acid ethyl ester |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN211358769U true CN211358769U (en) | 2020-08-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201921693681.9U Active CN211358769U (en) | 2019-10-11 | 2019-10-11 | Synthesis device of S-4-chloro-3-hydroxybutyric acid ethyl ester |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN211358769U (en) |
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2019
- 2019-10-11 CN CN201921693681.9U patent/CN211358769U/en active Active
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