N-Boc-L-valine purification device

By designing a combination of solvent extraction, recrystallization and chromatographic separation, the low efficiency problem of existing N-Boc-L-valine purification equipment was solved, an efficient and automated purification process was achieved, solvent waste and energy consumption were reduced, and production safety was ensured.

CN223366281UActive Publication Date: 2025-09-23NANJING ANHUAI INNOVATIVE PHARM RES INST CO LTD
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Patent Information

Application Number
CN202422783570.4
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-11-15
Publication Date
2025-09-23
Estimated Expiration
2034-11-15

AI Technical Summary

Technical Problem

The existing N-Boc-L-valine purification device has the problems of low purification efficiency, complex operation and incomplete solvent recovery.

Method used

A solvent extraction system, recrystallization device, chromatographic separation device and drying system were designed, combined with an agitator, vacuum filter, cooling device and safety device to achieve an efficient N-Boc-L-valine purification process.

Benefits of technology

It improves purification efficiency, reduces manual intervention, adapts to different specifications and purity requirements, reduces energy consumption and solvent waste, and ensures production safety.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses an N-Boc-L-valine purification device which comprises a solvent extraction system, a recrystallization device, a chromatographic separation device and a drying system, the solvent extraction system comprises a solvent extraction tank and a stirrer, the stirrer is arranged in the solvent extraction tank, a discharge valve is arranged at the bottom of the solvent extraction tank, and the recrystallization device is connected with the chromatographic separation device. The recrystallization device comprises a crystallization tank and a filtering system, a jacket is arranged outside the crystallization tank, the feeding end of the crystallization tank is connected with the solvent extraction tank, the discharging end of the crystallization tank is connected with the filtering system, the discharging end of the filtering system is connected with the chromatographic separation device, and the chromatographic separation device is further connected with the drying system. According to the device, the purity of N-Boc-L-valine can be effectively improved through the combination of solvent extraction, recrystallization and chromatographic separation. Due to the design of all the devices, the whole purification process is high in automation degree, manual intervention is reduced, and the production efficiency is improved.
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Description

Technical Field

[0001] The utility model relates to the technical field of chemical synthesis, and more specifically, to an N-Boc-L-valine purification device. Background Art

[0002] N-Boc-L-valine is an important amino acid derivative widely used in pharmaceutical and chemical synthesis. Its purification process typically involves multiple steps, including solvent extraction, recrystallization, and chromatographic separation. Existing purification devices suffer from several drawbacks, including low purification efficiency, complex operation, and incomplete solvent recovery. Therefore, there is an urgent need for an N-Boc-L-valine purification device with a rational structure, simple operation, and improved purification efficiency. Utility Model Content

[0003] The purpose of this utility model is to provide an N-Boc-L-valine purification device, aiming to address the low purification efficiency and complex operation problems of the existing technology. By designing a solvent extraction system, a recrystallization device, a chromatographic separation device, and a drying system, this device achieves a highly efficient N-Boc-L-valine purification process.

[0004] In order to achieve the above-mentioned purpose, the technical solution of the present utility model is as follows:

[0005] An N-Boc-L-valine purification device includes a solvent extraction system, a recrystallization device, a chromatographic separation device, and a drying system. The solvent extraction system includes a solvent extraction tank and an agitator. The agitator is located in the solvent extraction tank and generally uses a stirring paddle or a magnetic stirrer to ensure uniform mixing of the solution.

[0006] A discharge valve is provided at the bottom of the solvent extraction tank to completely discharge the solvent;

[0007] The recrystallization device includes a crystallization tank and a filtration system. A jacket is provided on the outside of the crystallization tank. The feed end of the crystallization tank is connected to the solvent extraction tank, the discharge end of the crystallization tank is connected to the filtration system, the discharge end of the filtration system is connected to a chromatographic separation device, and the chromatographic separation device is also connected to a drying system.

[0008] As an improvement of the present invention, a heat-conducting medium is provided in the jacket of the crystallization tank, and the crystallization tank is provided with a temperature control device, which can regulate the temperature of the crystallization tank by heating or cooling the heat-conducting medium.

[0009] As an improvement of the present invention, a cooling device is further provided outside the jacket of the crystallization tank, and the cooling device is a cooling coil or a cooling plate to ensure that the solution can reach the crystallization condition within a reasonable time.

[0010] As an improvement of the present invention, the filtration system is a vacuum filter or a centrifugal separator, which is used to separate the crystallized N-Boc-L-valine and the solvent.

[0011] As an improvement of the present invention, the chromatographic separation device includes a chromatographic column, a mobile phase storage tank, and a liquid recovery system. The chromatographic column separates different components of N-Boc-L-valine according to molecular weight or hydrophilicity. Furthermore, the chromatographic column is composed of multiple modules, each of which has a filler layer (such as silica gel) and separates the solutes through a mobile phase (such as water or an alcohol solvent);

[0012] The mobile phase storage tank is connected to the chromatographic column through a pipeline. Furthermore, a liquid distribution system can be set on the pipeline. The liquid recovery system is connected to the chromatographic column and uses gravity or a pump to return the reflux liquid to the storage tank for recovering the separated solvent and unseparated substances.

[0013] As an improvement of the present invention, the N-Boc-L-valine purification device further includes a safety device, which includes a pressure relief valve and an exhaust device, and the safety device is connected to the solvent extraction system.

[0014] The beneficial effects of the utility model are:

[0015] This device effectively improves the purity of N-Boc-L-valine through a combination of solvent extraction, recrystallization, and chromatographic separation. The design of each device enables a high degree of automation throughout the purification process, reducing manual intervention and improving production efficiency. Temperature and flow parameters can be adjusted according to actual production needs, adapting to production processes with varying specifications and purity requirements.

[0016] This device, through the design of a solvent recovery system and temperature control device, can effectively reduce energy consumption and solvent waste, meeting the requirements of green production. In addition, a pressure relief valve and exhaust device are designed to ensure the safety of the equipment during operation. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 This is a schematic structural diagram of the utility model.

[0018] List of Figure Symbols:

[0019] 1. Solvent extraction tank; 2. Discharge valve; 3. Crystallization tank; 4. Filtration system; 5. Chromatographic column; 6. Mobile phase storage tank; 7. Liquid recovery system; 8. Drying system; 9. Pressure relief valve; 10. Exhaust device; 31. Jacket; 32. Cooling device. DETAILED DESCRIPTION

[0020] The present invention will be further described below with reference to the accompanying drawings and specific embodiments. It should be understood that the following specific embodiments are intended only to illustrate the present invention and are not intended to limit the scope of the present invention. It should be noted that the terms "front," "rear," "left," "right," "up," and "down" used in the following description refer to directions in the accompanying drawings, and the terms "inward" and "outward" refer to directions toward or away from the geometric center of a particular component, respectively.

[0021] Furthermore, the terms "mounted," "connected," and "connected" should be interpreted broadly. For example, they can refer to fixed, detachable, or integral connections; mechanical or electrical connections; direct or indirect connections through an intermediary; and internal communication between two components. Those skilled in the art will understand the specific meanings of these terms in this utility model in their respective contexts.

[0022] As shown in the figure, the N-Boc-L-valine purification device described in the present invention includes a solvent extraction system, a recrystallization device, a chromatographic separation device, and a drying system 8. The solvent extraction system includes a solvent extraction tank 1 and an agitator. The agitator is disposed in the solvent extraction tank 1 and generally uses a stirring paddle or a magnetic stirrer to ensure uniform mixing of the solution.

[0023] A discharge valve 2 is provided at the bottom of the solvent extraction tank 1 to completely discharge the solvent;

[0024] The recrystallization device includes a crystallization tank 3 and a filtration system 4. A jacket 31 is provided on the outside of the crystallization tank 3. The feed end of the crystallization tank 3 is connected to the solvent extraction tank 1, and the discharge end of the crystallization tank 3 is connected to the filtration system 4. The discharge end of the filtration system 4 is connected to a chromatographic separation device, and the chromatographic separation device is also connected to a drying system 8.

[0025] The jacket 31 of the crystallization tank 3 of the present invention is provided with a heat-conducting medium. The crystallization tank 3 is provided with a temperature control device, which can regulate the temperature of the crystallization tank 3 by heating or cooling the heat-conducting medium.

[0026] The jacket 31 of the crystallization tank 3 of the present invention is further provided with a cooling device 32 outside thereof. The cooling device 32 is a cooling coil or a cooling plate, which ensures that the solution can reach the crystallization condition within a reasonable time.

[0027] The filtration system 4 described in the present invention is a vacuum filter or a centrifugal separator, which is used to separate the crystallized N-Boc-L-valine and the solvent.

[0028] The chromatographic separation device described in the present invention includes a chromatographic column 5, a mobile phase storage tank 6, and a liquid recovery system 7. The chromatographic column 5 separates different components of N-Boc-L-valine according to molecular weight or hydrophilicity. Furthermore, the chromatographic column 5 is composed of multiple modules, each of which has a filler layer (such as silica gel) and separates the solutes through a mobile phase (such as water or an alcohol solvent);

[0029] The mobile phase storage tank 6 is connected to the chromatographic column 5 through a pipeline. Furthermore, a liquid distribution system can be set on the pipeline. The liquid recovery system 7 is connected to the chromatographic column 5 and uses gravity or a pump to return the reflux liquid to the storage tank for recovering the separated solvent and unseparated substances.

[0030] The N-Boc-L-valine purification device of the present invention further comprises a safety device, which comprises a pressure relief valve 9 and an exhaust device 10, and the safety device is connected to the solvent extraction system.

[0031] The working principle of the N-Boc-L-valine purification device described in the utility model is:

[0032] (1) Solvent extraction: N-Boc-L-valine is added to the solvent extraction tank 1. After the agitator is started, the solvent and N-Boc-L-valine are fully mixed to form a solution. The solution is transported to the recrystallization device through a pipeline.

[0033] (2) Recrystallization: The solution enters the crystallization tank 3, where the temperature is adjusted by the heat-conducting medium in the jacket 31 to promote the crystallization of N-Boc-L-valine. The crystallized solution passes through the filtration system 4 for solid-liquid separation, and impurities are filtered out.

[0034] (3) Chromatographic separation: The crystallized solution is further separated by a chromatographic separation device. The mobile phase flows from the storage tank into the chromatographic column 5. When passing through the chromatographic column 5, N-Boc-L-valine is effectively separated. The separated solvent and impurities are refluxed through the liquid recovery system 7.

[0035] (4) Drying treatment: The separated pure N-Boc-L-valine enters the drying system 8, where excess solvent and moisture are removed by vacuum heating to obtain the final high-purity product.

[0036] The pressure during the whole process is controlled by the relief valve and the exhaust device 10 to ensure the safe operation of the device.

[0037] Through the above work flow, the device can efficiently and stably complete the purification process of N-Boc-L-valine, ensuring the quality of the product and the safety of production.

[0038] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that includes a list of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus.

[0039] The accompanying drawings merely illustrate the technical concept of the present invention and cannot limit the scope of protection of the present invention by this shape. For ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications all fall within the scope of protection of the claims of the present invention.

Claims

1. An N-Boc-L-valine purification device, comprising a solvent extraction system, a recrystallization device, a chromatographic separation device, and a drying system, characterized in that: The solvent extraction system includes a solvent extraction tank and an agitator, wherein the agitator is arranged in the solvent extraction tank, a discharge valve is provided at the bottom of the solvent extraction tank, the recrystallization device includes a crystallization tank and a filtration system, a jacket is provided on the outside of the crystallization tank, the feed end of the crystallization tank is connected to the solvent extraction tank, the discharge end of the crystallization tank is connected to the filtration system, the discharge end of the filtration system is connected to a chromatographic separation device, and the chromatographic separation device is also connected to a drying system.

2. The N-Boc-L-valine purification device according to claim 1, characterized in that: A heat-conducting medium is provided in the jacket of the crystallization tank, and the crystallization tank is provided with a temperature control device, which can regulate the temperature of the crystallization tank by heating or cooling the heat-conducting medium.

3. The N-Boc-L-valine purification device according to claim 2, characterized in that: A cooling device is further provided outside the jacket of the crystallization tank, and the cooling device is a cooling coil or a cooling plate.

4. The N-Boc-L-valine purification device according to claim 2, characterized in that: The filtration system is a vacuum filter or a centrifugal separator.

5. The N-Boc-L-valine purification device according to claim 1, characterized in that: The chromatographic separation device comprises a chromatographic column, a mobile phase storage tank, and a liquid recovery system. The mobile phase storage tank is connected to the chromatographic column through a pipeline, and the liquid recovery system is connected to the chromatographic column.

6. The N-Boc-L-valine purification device according to claim 1, characterized in that: The N-Boc-L-valine purification device further comprises a safety device, which comprises a pressure relief valve and an exhaust device, and the safety device is connected to the solvent extraction system.