CN221208079U - 3- (4-Fluorophenyl) -1-isopropyl-1H-indole production system - Google Patents
3- (4-Fluorophenyl) -1-isopropyl-1H-indole production system Download PDFInfo
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- CN221208079U CN221208079U CN202323179393.0U CN202323179393U CN221208079U CN 221208079 U CN221208079 U CN 221208079U CN 202323179393 U CN202323179393 U CN 202323179393U CN 221208079 U CN221208079 U CN 221208079U
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- Prior art keywords
- kettle
- mother liquor
- pipeline
- desolventizing
- hydrolysis
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- ZDZJOIIBECYKAJ-UHFFFAOYSA-N 3-(4-fluorophenyl)-1-propan-2-ylindole Chemical compound C12=CC=CC=C2N(C(C)C)C=C1C1=CC=C(F)C=C1 ZDZJOIIBECYKAJ-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- 239000012452 mother liquor Substances 0.000 claims abstract description 38
- 238000002425 crystallisation Methods 0.000 claims abstract description 37
- 230000008025 crystallization Effects 0.000 claims abstract description 37
- 230000007062 hydrolysis Effects 0.000 claims abstract description 32
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 32
- 239000000047 product Substances 0.000 claims abstract description 32
- 238000000926 separation method Methods 0.000 claims abstract description 30
- 239000002904 solvent Substances 0.000 claims abstract description 30
- 238000000605 extraction Methods 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 210000003298 dental enamel Anatomy 0.000 claims abstract description 7
- 239000013067 intermediate product Substances 0.000 claims abstract description 3
- 238000011084 recovery Methods 0.000 claims description 29
- 239000012043 crude product Substances 0.000 claims description 9
- 239000012074 organic phase Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012071 phase Substances 0.000 claims description 6
- 239000010865 sewage Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000001953 recrystallisation Methods 0.000 claims description 2
- 238000012824 chemical production Methods 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- VGCXGMAHQTYDJK-UHFFFAOYSA-N Chloroacetyl chloride Chemical compound ClCC(Cl)=O VGCXGMAHQTYDJK-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- FJLGEFLZQAZZCD-MCBHFWOFSA-N (3R,5S)-fluvastatin Chemical compound C12=CC=CC=C2N(C(C)C)C(\C=C\[C@@H](O)C[C@@H](O)CC(O)=O)=C1C1=CC=C(F)C=C1 FJLGEFLZQAZZCD-MCBHFWOFSA-N 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229960003765 fluvastatin Drugs 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to the field of chemical production, and provides a 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system. Including first main reation kettle and second main reation kettle, first main reation kettle top is connected with two dropwise add jars, simultaneously to the first interior dropwise add raw materials of main reation kettle, first main reation kettle's bottom has first hydrolysis kettle through enamel pipe connection, extraction cauldron is connected to first hydrolysis kettle, extraction kettle connects desolventizing cauldron, the intermediate product after desolventizing in the desolventizing cauldron gets into second main reation kettle through the pipeline, second main reation kettle is connected with the second and hydrolyzes the cauldron, the crystallization separator is connected through the transfer cauldron to the second hydrolysis kettle. The system firstly prepares the intermediate and recovers the solvent, ensures the purity of the intermediate, then prepares a final finished product by taking the intermediate as a raw material, ensures that the finished product can be completely separated from the mother liquor through twice crystallization and centrifugal separation after reaction and hydrolysis of the intermediate, improves the yield, recovers the mother liquor and the solvent therein for secondary use, and reduces the production cost.
Description
Technical Field
The utility model relates to the field of chemical production, in particular to a 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system.
Background
3- (4-Fluorophenyl) -1-isopropyl-1H-indole is an intermediate for use as the drug fluvastatin, the finished product of which is a white or pale green solid. The preparation process includes quenching and phase separating to obtain intermediate, reaction of the intermediate with anhydrous alcohol as solvent and N-isopropyl amine, hydrolysis, crystallization and centrifugal separation to obtain the product.
In the reaction process, an intermediate is needed to be prepared, then the intermediate is used as a raw material to prepare a finished product, solvents used in two reaction stages are different, the solvents are needed to be recovered in the respective stages, and the separation difficulty caused by the mixing of the solvents is avoided. The final finished product is separated out in a solid form through crystallization and centrifugal separation, mother liquor can be used mechanically, and the finished product in the mother liquor is required to be separated in order to ensure the yield of the final finished product and the quality of the mother liquor.
Disclosure of utility model
In order to ensure the yield of the finished products of 3- (4-fluorophenyl) -1-isopropyl-1H-indole and ensure the application of various solvents and mother liquor, the utility model aims to provide a 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system.
The technical scheme adopted by the utility model is as follows:
The 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system comprises a first main reaction kettle and a second main reaction kettle, wherein the top of the first main reaction kettle is connected with two dripping tanks, raw materials are dripped into the first main reaction kettle at the same time, the bottom of the first main reaction kettle is connected with a first hydrolysis kettle through a enamel pipe, the bottom of the first hydrolysis kettle is provided with a sewage discharge pipe and a pipeline connected with an extraction kettle, the water phase in the first hydrolysis kettle is discharged and treated, an organic phase in the first hydrolysis kettle enters the extraction kettle, the bottom of the extraction kettle is provided with a sewage discharge pipe and a pipeline connected with a desolventizing kettle, the water phase in the extraction kettle is discharged and treated, the organic phase returns to the hydrolysis kettle or enters a desolventizing kettle, and a gas outlet at the top of the desolventizing kettle is connected with a first solvent recovery tank through a condenser; intermediate products after desolventizing in the desolventizing kettle enter a second main reaction kettle through a pipeline, the bottom of the second main reaction kettle is connected with a second hydrolysis kettle through an enamel pipeline, the bottom of the second hydrolysis kettle is connected with a first centrifugal separator through a pipeline, solid crude products in the first centrifugal separator are sent into a transfer kettle and dissolved through a solvent, and the dissolved crude products in the transfer kettle are separated into finished products through a crystallization separation device.
Further, the crystallization separation device comprises a two-stage crystallization separation unit, the crystallization separation unit comprises a crystallization kettle, a centrifugal separator and a mother liquor recovery kettle, a crude product in the transfer kettle is transferred into the crystallization kettle of the first-stage crystallization separation unit through a pipeline, mixed liquor after cooling crystallization enters the centrifugal separator for separation, separated solids are collected and dried to obtain a finished product, and separated mother liquor enters the mother liquor recovery kettle through the pipeline; and (3) enabling the mother liquor in the mother liquor recovery kettle to enter a crystallization kettle of the secondary crystallization separation unit through a pipeline for recrystallization, enabling the crystallized mixed liquor to enter a centrifugal separator for secondary separation, collecting and drying the separated solids to obtain a finished product, and enabling the separated mother liquor to enter the corresponding mother liquor recovery kettle.
Further, the top of the mother liquor recovery kettle is connected with a condenser, and the mother liquor recovery kettle evaporates the solvent in the mother liquor and enters a second solvent recovery tank after being condensed by the condenser.
Further, the organic phase is input into the two desolventizing kettles arranged in parallel through a branch pipeline and a control box of a valve at the bottom of the extraction kettle, and the two desolventizing kettles share a first solvent recovery tank.
Further, the reactor comprises two parallel second main reaction kettles.
Further, a pipeline connected with the top of the first hydrolysis kettle is arranged at the bottom of the extraction kettle.
Further, an exhaust pipeline is arranged at the top of the first main reaction kettle and is connected with a tail gas treatment station.
After the technical scheme is adopted, the beneficial effects of the utility model are as follows:
The system firstly prepares the intermediate and recovers the solvent in the intermediate, ensures the purity of the intermediate, then prepares a final finished product by taking the intermediate as a raw material, ensures that the finished product can be completely separated from the mother liquor after reaction and hydrolysis and through twice crystallization and centrifugal separation, improves the yield of the finished product, recovers and reutilizes the mother liquor and the solvent therein, and reduces the production cost.
Drawings
FIG. 1 is a diagram of a production system for an intermediate.
Fig. 2 is a diagram of a production system of the finished product.
In the figure: the device comprises a first main reaction kettle 1, a chloroacetyl chloride dropwise adding tank 2, a fluorobenzene dropwise adding tank 3, a first hydrolysis kettle 4, an extraction kettle 5, a desolventizing kettle 6, a first solvent recycling tank 7, a second main reaction kettle 8, a second hydrolysis kettle 9, a first centrifugal separator 10, a transfer kettle 11, a crystallization kettle 12, a second centrifugal separator 13, a mother liquor recycling kettle 14 and a second solvent recycling tank 15.
Detailed Description
The following detailed description of the utility model refers to the accompanying drawings, which illustrate specific embodiments of the utility model:
As shown in FIG. 1, a 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system consists of an intermediate preparation unit and a finished product preparation unit. The intermediate prepared by the intermediate preparation unit is used as a raw material to prepare a finished product in the finished product preparation unit, and the finished product is subjected to hydrolysis, crystallization and centrifugal separation to obtain the finished product.
The intermediate preparation unit consists of a first main reaction kettle 1, a chloroacetyl chloride dropwise adding tank 2, a fluorobenzene dropwise adding tank 3, a first hydrolysis kettle 4, an extraction kettle 5, a desolventizing kettle 6, a first solvent recovery tank 7 and related pipelines and valves. The solvent methylene dichloride and the anhydrous aluminum trichloride serving as a catalyst are added into the first main reaction kettle 1, raw materials are dropwise added into the first main reaction kettle 1 from a chloroacetyl chloride dropwise adding tank 2 and a fluorobenzene dropwise adding tank 3, the reaction is kept for 5 hours after the dropwise adding is finished, and the reaction is finished when the fluorobenzene content is detected to be less than 2%. The top of the first main reaction kettle 1 is provided with an exhaust pipeline which is connected with a tail gas treatment station.
The mixed solution after the reaction is controlled to enter a first hydrolysis kettle 4 through a enamel pipe and a valve, is quenched by adding hydrochloric acid solution, is kept stand and layered, then a lower water phase is discharged and treated through a sewage discharge pipe, an upper organic phase enters an extraction kettle 5 through a pipeline, after three times of water washing, water and a water-soluble catalyst in the organic phase are discharged and treated through a sewage discharge pipe at the bottom of the extraction kettle 5, the organic phase enters a desolventizing kettle 6 through a pipeline or returns to the first hydrolysis kettle 4 for continuous hydrolysis, the technical scheme is provided with two parallel desolventizing kettles 6, the desolventizing kettles 6 are heated, solvent dichloromethane in the desolventizing kettle is evaporated and condensed and liquefied through a condenser at the top of the desolventizing kettle, and then enters a first solvent recovery tank 7 for recycling, and the two desolventizing kettles 6 share the first solvent recovery tank 7. The rest in the desolventizing kettle 6 is an intermediate.
The finished product preparation unit consists of a second main reaction kettle 8, a second hydrolysis kettle 9, a first centrifugal separator 10, a transfer kettle 11, a crystallization separation device and related pipelines and valves.
The intermediate after desolventizing in the desolventizing kettle 6 enters a second main reaction kettle 8 through a pipeline, two parallel second main reaction kettles are arranged in the technical scheme, absolute ethyl alcohol serving as a solvent, absolute zinc chloride serving as a catalyst and N-isopropylamine serving as a raw material are added in the second main reaction kettle 8, the temperature is raised to 105-115 ℃ to keep the reaction for 15 hours, the reaction is completed when the content of the intermediate is detected to be less than 1%, the temperature is lowered to 40-50 ℃, the material enters a second hydrolysis kettle 9 through an enamel pipeline, hydrochloric acid aqueous solution is added in the second hydrolysis kettle 9, after stirring for 1 hour, the mixed solution is sent into a first centrifugal separator 10, the aqueous solution, the catalyst and the like are separated, the rest crude product enters a transfer kettle 11 through a pipeline, absolute ethyl alcohol is added in the transfer kettle 11, the stirring is carried out, the temperature is raised to 78-85 ℃ to enable the crude product to be completely dissolved, and the transfer kettle 11 sends the dissolved material into a crystallization separation device through a pipeline and a pump to separate the finished product.
The crystallization separation device comprises two stages of crystallization separation units connected in series. The crystallization separation unit is composed of a crystallization kettle 12, a second centrifugal separator 13, a mother liquor recovery kettle 14 and a second solvent recovery tank 15. The crude product solution in the transfer kettle 11 enters a crystallization kettle 12 of a first-stage crystallization separation device, the temperature is reduced to 20 ℃ to crystallize the finished product, the crystallized finished product enters a second centrifugal separator 13 for separation, the separated mother liquor enters a mother liquor recovery kettle 14, and the separated solid wet product is decompressed and dried at 40 ℃ to obtain the finished product. Mother liquor in the mother liquor recovery kettle 14 enters the second-stage crystallization separation device through a pipeline to carry out secondary crystallization separation, so that finished products in the mother liquor can be separated, and the yield of the finished products is ensured.
The mother liquor recovery kettle 14 is heated, the ethanol in the mother liquor recovery kettle is evaporated and condensed by a condenser at the top of the mother liquor recovery kettle, and the condensed ethanol enters the second solvent recovery tank 15 and can be reused.
Claims (7)
1. The 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system comprises a first main reaction kettle and a second main reaction kettle, and is characterized in that the top of the first main reaction kettle is connected with two dropping tanks, raw materials are simultaneously dropped into the first main reaction kettle, the bottom of the first main reaction kettle is connected with a first hydrolysis kettle through a enamel pipe, the bottom of the first hydrolysis kettle is provided with a sewage discharge pipe and a pipeline connected with an extraction kettle, the water phase in the first hydrolysis kettle is discharged and treated, an organic phase in the first hydrolysis kettle enters the extraction kettle, the bottom of the extraction kettle is provided with a sewage discharge pipe and a pipeline connected with a desolventizing kettle, the water phase in the extraction kettle is discharged and treated, the organic phase returns to the hydrolysis kettle or enters the desolventizing kettle, and a gas outlet at the top of the desolventizing kettle is connected with a first solvent recovery tank through a condenser; intermediate products after desolventizing in the desolventizing kettle enter a second main reaction kettle through a pipeline, the bottom of the second main reaction kettle is connected with a second hydrolysis kettle through an enamel pipeline, the bottom of the second hydrolysis kettle is connected with a first centrifugal separator through a pipeline, solid crude products in the first centrifugal separator are sent into a transfer kettle and dissolved through a solvent, and the dissolved crude products in the transfer kettle are separated into finished products through a crystallization separation device.
2. The 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system according to claim 1, wherein the crystallization separation device comprises a two-stage crystallization separation unit, the crystallization separation unit comprises a crystallization kettle, a centrifugal separator and a mother liquor recovery kettle, a crude product in the transfer kettle is transferred into the crystallization kettle of the first-stage crystallization separation unit through a pipeline, a mixed liquor after cooling crystallization enters the centrifugal separator to be separated, separated solids are collected and dried to obtain a finished product, and separated mother liquor enters the mother liquor recovery kettle through a pipeline; and (3) enabling the mother liquor in the mother liquor recovery kettle to enter a crystallization kettle of the secondary crystallization separation unit through a pipeline for recrystallization, enabling the crystallized mixed liquor to enter a centrifugal separator for secondary separation, collecting and drying the separated solids to obtain a finished product, and enabling the separated mother liquor to enter the corresponding mother liquor recovery kettle.
3. The 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system according to claim 2, wherein the top of the mother liquor recovery kettle is connected with a condenser, and the mother liquor recovery kettle evaporates the solvent in the mother liquor and condenses the solvent by the condenser and then enters the second solvent recovery tank.
4. The 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system according to claim 1, comprising two desolventizing kettles arranged in parallel, wherein an organic phase is input into the two desolventizing kettles at the bottom of the extraction kettle through a branch pipeline and a control box of a valve, and the two desolventizing kettles share a first solvent recovery tank.
5. A 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system according to claim 1, comprising two second main reaction vessels side by side.
6. The 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system according to claim 1, wherein the bottom of the extraction kettle is provided with a pipeline connected to the top of the first hydrolysis kettle.
7. The 3- (4-fluorophenyl) -1-isopropyl-1H-indole production system according to claim 1, wherein an exhaust pipeline is arranged at the top of the first main reaction kettle and is connected with an exhaust gas treatment station.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202323179393.0U CN221208079U (en) | 2023-11-24 | 2023-11-24 | 3- (4-Fluorophenyl) -1-isopropyl-1H-indole production system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202323179393.0U CN221208079U (en) | 2023-11-24 | 2023-11-24 | 3- (4-Fluorophenyl) -1-isopropyl-1H-indole production system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN221208079U true CN221208079U (en) | 2024-06-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202323179393.0U Active CN221208079U (en) | 2023-11-24 | 2023-11-24 | 3- (4-Fluorophenyl) -1-isopropyl-1H-indole production system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN221208079U (en) |
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2023
- 2023-11-24 CN CN202323179393.0U patent/CN221208079U/en active Active
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