CN212476591U - Production system of homotaurine - Google Patents
Production system of homotaurine Download PDFInfo
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- CN212476591U CN212476591U CN202020950193.8U CN202020950193U CN212476591U CN 212476591 U CN212476591 U CN 212476591U CN 202020950193 U CN202020950193 U CN 202020950193U CN 212476591 U CN212476591 U CN 212476591U
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Abstract
The utility model relates to a high taurine's production system, including mercaptan acetate reation kettle, mercaptan acetate reation kettle pan feeding mouth passes through pipeline and 2-butene amide storage tank, dichloromethane storage tank and triethylamine storage tank communicate respectively, mercaptan ester reation kettle bottom bin outlet passes through pipeline and chromatographic fractionation ware, mercaptan acetate dilution jar communicates in proper order, mercaptan acetate dilution jar discharge gate passes through pipeline and aminopropanethiol retort intercommunication, aminopropanol retort pan feeding mouth passes through pipeline and aluminium hydride lithium storage tank intercommunication, aminopropanol reation tank bottom discharge gate passes through pipeline and filter intercommunication, the filtrating discharge gate of filter passes through pipeline and extraction jar, peroxyformic acid oxidation tank and recrystallization jar communicate in proper order. The utility model discloses a 2-butenamide, thioacetic acid take place addition reaction, and the reduction of rethread aluminium lithium hydride obtains high taurine through formic acid, hydrogen peroxide oxidation at last, and the raw materials economy is easily obtained, has reduced manufacturing cost.
Description
Technical Field
The utility model relates to a chemical synthesis technical field relates to homotaurine's production system.
Background
The homotaurine is sulfamic acid separated from Grateloupia livida, is named as 3-amino-1-propanesulfonic acid, and is a taurine derivative with one more carbon on a carbon chain. Because of having certain curative effect on Alzheimer's disease and hemorrhagic apoplexy, people pay more attention to the treatment. Due to their potential pharmaceutical value, new synthetic methods are continually being investigated. The following is a method for synthesizing homotaurine reported so far. The synthesis method of 3-amino-1-propanesulfonic acid is still less, and the method for preparing 3-aminopropanesulfonic acid by CN03117659.3 discloses that: introducing hydrogen chloride gas into 3-aminopropanol as raw material until absorption is stopped, adding ethanol for dilution, cooling and crystallizing to obtain intermediate compound, preparing the separated intermediate compound into aqueous solution, carrying out sulfonation reaction with aqueous solution of alkali metal sulfite under reflux, acidifying with hydrochloric acid after reaction, filtering while hot, cooling and crystallizing to obtain the 3-aminopropanesulfonic acid product. But the reaction reagent is expensive and the cost is high. The raw materials are not easy to prepare, and the position and the type of the substituent group are greatly limited.
Disclosure of Invention
In order to solve the technical problem, the utility model provides a production system of homotaurine adopts 2-butene amide, through taking place addition reaction with thioacetic acid, and the rethread lithium aluminium hydride reduction obtains amino mercaptan compound, and the hydrogen peroxide oxidation obtains homotaurine, and the raw materials economy is easy, has reduced homotaurine's manufacturing cost.
The scheme of the utility model is that:
a production system of high taurine comprises a mercaptan acetate reaction kettle, wherein a material inlet of the mercaptan acetate reaction kettle is respectively communicated with a 2-butenamide storage tank, a dichloromethane storage tank and a triethylamine storage tank through pipelines, a first radiator and a first condenser are sequentially arranged above the mercaptan ester reaction kettle, a material outlet of the first condenser is communicated with the mercaptan ester reaction kettle through a pipeline to form a backflow pipeline, a material outlet at the bottom of the mercaptan ester reaction kettle is sequentially communicated with a chromatographic separator and a mercaptan acetate dilution tank through pipelines, a material outlet of the mercaptan acetate dilution tank is communicated with an aminopropanethiol reaction tank through a pipeline, a material inlet of the aminopropanethiol reaction tank is communicated with an aluminum hydride storage tank through a pipeline, a second radiator and a second condenser are sequentially arranged above the top of the aminopropanethiol reaction tank, a material outlet at the bottom of the second condenser is communicated with the aminopropanethiol reaction tank through a pipeline, the discharge port at the bottom of the aminopropanethiol reaction tank is communicated with a filter through a pipeline, and the filtrate discharge port of the filter is sequentially communicated with an extraction tank, a peroxyformic acid oxidation tank and a recrystallization tank through pipelines.
Preferably, the bottom of the thiol ester reaction kettle is provided with a nitrogen inlet pipe.
Preferably, the surfaces of the aminopropanethiol reaction tank, the lithium aluminum hydride storage tank and the peroxyformic acid oxidation tank are provided with interlayers, and the interlayers are respectively connected with the cooling medium generator through pipelines.
Preferably, the discharge port of the first condenser is also communicated with a condensate recovery tank through a pipeline.
Preferably, the mercaptan acetate dilution tank is provided with a tetrahydrofuran addition line.
Preferably, the extraction tank is provided with a dichloromethane input pipe communicated with a dichloromethane storage tank.
Preferably, the peroxyformic acid oxidation tank is provided with a formic acid input pipe and a hydrogen peroxide input pipe.
Preferably, the recrystallization tank is provided with an ethanol input pipe.
Preferably, the interlayer is in communication with the medium cooler and the medium heater through pipes, respectively.
The utility model discloses beneficial effect:
1. the utility model discloses an adopt 2-butenamide, through taking place addition reaction with thioacetic acid, obtain corresponding acetic acid carbamoyl alkyl mercaptan ester midbody, amino mercaptan compound is obtained in the reduction of rethread aluminium hydride lithium, obtains homotaurine through formic acid, hydrogen peroxide oxidation at last, and the raw materials economy is easily obtained, has reduced homotaurine's manufacturing cost.
2. The bottom of the mercaptan ester reaction kettle is provided with a nitrogen inlet pipe, the surfaces of the aminopropanethiol reaction tank, the lithium aluminum hydride storage tank and the peroxyformic acid oxidation tank are provided with interlayers, and the interlayers are respectively connected with a cooling medium generator through pipelines, so that byproducts generated in the reaction are prevented, and the product yield is improved.
3. The discharge port of the first condenser is also fully refluxed with the condensate recovery tank through a pipeline. The mercaptan acetate ester diluting tank is provided with a tetrahydrofuran adding pipe and is used for diluting mercaptan acetate ester.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention;
wherein: the device comprises a mercaptan acetate reaction kettle 1, a mercaptan acetate reaction kettle 2-butenamide storage tank 3, a dichloromethane storage tank 4, a triethylamine storage tank 5, a nitrogen inlet pipe 6, a first radiator 7, a first condenser 8, a chromatographic separator 9, a mercaptan acetate dilution tank 10, an aminopropanethiol reaction tank 11, an aluminum lithium hydride storage tank 12, a second radiator 13, a second condenser 14, a filter 15, an extraction tank 16, a peroxyformic acid oxidation tank 17, a recrystallization tank 18, a cooling medium generator 19 and a condensate recovery tank 20.
Detailed Description
The invention is further described with reference to the following examples, but the scope of the invention as claimed is not limited to the scope of the examples.
Example 1
A production system of high taurine comprises a mercaptan acetate reaction kettle 1, a feeding port of the mercaptan acetate reaction kettle 1 is respectively communicated with a 2-butenamide storage tank 3, a dichloromethane storage tank 4 and a triethylamine storage tank 5 through pipelines, a first radiator 7 and a first condenser 8 are sequentially arranged above the mercaptan ester reaction kettle 1, a discharging port of the first condenser 8 is communicated with the mercaptan ester reaction kettle 1 through a pipeline to form a backflow pipeline, a discharging port at the bottom of the mercaptan ester reaction kettle 1 is sequentially communicated with a chromatographic separator 9 and a mercaptan acetate dilution tank 10 through pipelines, a discharging port of the mercaptan acetate dilution tank 10 is communicated with an aminopropanethiol reaction tank 11 through a pipeline, a feeding port of the aminopropanol reaction tank 11 is communicated with an aluminum hydride storage tank 12 through a pipeline, a second radiator 13 and a second condenser 14 are sequentially arranged above the top of the aminopropanol reaction tank 11, a discharging port at the bottom of the second condenser 14 is communicated with the aminopropanol reaction tank 11 through a pipeline, the discharge port at the bottom of the aminopropanethiol reaction tank 11 is communicated with a filter 15 through a pipeline, and the filtrate discharge port of the filter 15 is sequentially communicated with an extraction tank 16, a peroxyformic acid oxidation tank 17 and a recrystallization tank 18 through pipelines.
Preferably, the bottom of the thiol ester reaction kettle 1 is provided with a nitrogen inlet pipe 6.
Preferably, the surfaces of the aminopropanethiol reaction tank 11, the lithium aluminum hydride storage tank 12 and the peroxyformic acid oxidation tank 17 are provided with interlayers, and the interlayers are respectively connected with the cooling medium generator 19 through pipelines.
Preferably, the discharge port of the first condenser 8 is also communicated with a condensate recovery tank 20 through a pipeline.
Preferably, the mercaptan acetate dilution tank 10 is provided with a tetrahydrofuran addition line.
Preferably, the extraction tank 16 is provided with a dichloromethane input pipe communicated with the dichloromethane storage tank 4.
Preferably, the peroxyformic acid oxidation tank 17 is provided with a formic acid input pipe and a hydrogen peroxide input pipe.
Preferably, the recrystallization tank 18 is provided with an ethanol input pipe.
The utility model discloses during the use: the medium generated by the cooling medium generator 19 is ice water with the temperature of 0 ℃,
cooling medium is introduced into an interlayer in a mercaptan acetate reaction kettle 1, and 2-butenamide and CH are sequentially input from a dichloromethane storage tank 4, a 2-butenamide storage tank 3 and a triethylamine storage tank 52Cl2And anhydrous triethylamine is added into a mercaptan acetate reaction kettle 1, nitrogen is introduced into the mercaptan acetate reaction kettle 1 for protection, heating reflux is carried out, thioacetic acid is dropwise added, reflux is carried out for 15-25 hours, and the solid-liquid ratio of 2-butenamide to dichloromethane is 0.85: 15 (g/mL), the molar ratio of 2-butenamide to thioacetic acid was 0.85: 0.95. cooling to room temperature, andthe reaction product is sent to a chromatographic separator 9 for separation to obtain an intermediate mercaptan acetate. Putting the mercaptane acetate into a mercaptane acetate diluting tank 10, diluting the mercaptane acetate with tetrahydrofuran, putting the mercaptane acetate into an aminopropanethiol reaction tank 11 for reaction, adding lithium aluminum hydride in a lithium aluminum hydride storage tank 12 into anhydrous tetrahydrofuran in ice-water bath, then adding the mixture into the aminopropanethiol reaction tank 11, heating and refluxing for 15-20h, wherein the solid-to-liquid ratio of the lithium aluminum hydride to the tetrahydrofuran is 1.53: 30 (g/m L), the molar ratio of aminopropanethiol lithium aluminum hydride being 1: 10. after the temperature is returned to room temperature, the mixture is quenched by water in an ice water bath, and water is added and stirred for 12 hours. Filtering in a filter 15, extracting the filtrate in an extraction tank 16 for five times by using dichloromethane, and removing the solvent to obtain the aminopropanethiol. Formic acid, aminopropanethiol and peroxyformic acid (the volume ratio of formic acid to 30% hydrogen peroxide is 5: 1) are sequentially added into a peroxyformic acid oxidation tank 17, and the ratio of aminopropanethiol: formic acid: the solid-to-liquid ratio of the peroxyformic acid is 0.34: 10: and 12, stirring at normal temperature overnight, putting into a recrystallization tank 18, and recrystallizing with ethanol to obtain the homotaurine.
The above-mentioned embodiments only represent the preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several changes, modifications and substitutions can be made, which are all within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
Claims (8)
1. A production system of homotaurine comprises a mercaptan acetate reaction kettle (1) and is characterized in that: a material inlet of a mercaptan acetate reaction kettle (1) is communicated with a 2-butenamide storage tank (3), a dichloromethane storage tank (4) and a triethylamine storage tank (5) through pipelines respectively, a first radiator (7) and a first condenser (8) are sequentially arranged above the mercaptan ester reaction kettle (1), a material outlet of the first condenser (8) is communicated with the mercaptan ester reaction kettle (1) through pipelines to form a backflow pipeline, a material outlet at the bottom of the mercaptan ester reaction kettle (1) is sequentially communicated with a chromatographic separator (9) and a mercaptan acetate dilution tank (10), a material outlet of the mercaptan acetate dilution tank (10) is communicated with an aminopropanethiol reaction tank (11) through pipelines, a material inlet of the aminopropanol reaction tank (11) is communicated with a lithium aluminum hydride storage tank (12) through a pipeline, a second radiator (13) and a triethylamine are sequentially arranged above the top of the aminopropanol reaction tank (11), The bottom discharge port of the second condenser (14) is communicated with the aminopropanethiol reaction tank (11) through a pipeline, the bottom discharge port of the aminopropanethiol reaction tank (11) is communicated with the filter (15) through a pipeline, and the filtrate discharge port of the filter (15) is sequentially communicated with the extraction tank (16), the peroxyformic acid oxidation tank (17) and the recrystallization tank (18) through pipelines.
2. The system for producing homotaurine according to claim 1, wherein: and a nitrogen inlet pipe (6) is arranged at the bottom of the thiol ester reaction kettle (1).
3. The system for producing homotaurine according to claim 1, wherein: interlayers are arranged on the surfaces of the aminopropanethiol reaction tank (11), the lithium aluminum hydride storage tank (12) and the peroxyformic acid oxidation tank (17), and are respectively connected with a cooling medium generator (19) through pipelines.
4. The system for producing homotaurine according to claim 1, wherein: the discharge hole of the first condenser (8) is also communicated with a condensate recovery tank (20) through a pipeline.
5. The system for producing homotaurine according to claim 1, wherein: the mercaptan acetate diluting tank (10) is provided with a tetrahydrofuran adding pipe.
6. The system for producing homotaurine according to claim 1, wherein: and a dichloromethane input pipe arranged in the extraction tank (16) is communicated with the dichloromethane storage tank (4).
7. The system for producing homotaurine according to claim 1, wherein: the peroxyformic acid oxidation tank (17) is provided with a formic acid input pipe and a hydrogen peroxide input pipe.
8. The system for producing homotaurine according to claim 1, wherein: the recrystallization tank (18) is provided with an ethanol input pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020950193.8U CN212476591U (en) | 2020-05-29 | 2020-05-29 | Production system of homotaurine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020950193.8U CN212476591U (en) | 2020-05-29 | 2020-05-29 | Production system of homotaurine |
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| Publication Number | Publication Date |
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| CN212476591U true CN212476591U (en) | 2021-02-05 |
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| CN202020950193.8U Active CN212476591U (en) | 2020-05-29 | 2020-05-29 | Production system of homotaurine |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: Production system of high taurine Effective date of registration: 20220927 Granted publication date: 20210205 Pledgee: Bank of China Limited by Share Ltd. Three Gorges Branch Pledgor: HUBEI GUANGCHEN PHARMACEUTICAL CO.,LTD. Registration number: Y2022420000330 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |