Device for preparing 5-fluoro-4, 6-dichloropyrimidine

Abstract

The utility model discloses a device for preparing 5-fluoro-4, 6-dichloropyrimidine, which comprises a head tank, a reaction kettle, a rectifying tower, a condenser, a vacuum pump, a first receiving tank, a second receiving tank and a third receiving tank, a feed port of the head tank is used for receiving dichloroethane and phosphorus oxychloride, and a discharge port of the head tank is connected with a first feed port of the reaction kettle; the reaction kettle is further provided with a feeding port used for feeding dihydroxypyrimidine, a discharging port of the reaction kettle is connected with a feeding port of the rectifying tower, the rectifying tower is connected with a condenser, and the condenser is connected with a vacuum pump. A discharging port of the rectifying tower is connected with a feeding port of a first receiving tank, a feeding port of a second receiving tank and a feeding port of a third receiving tank through a first pipeline, a second pipeline and a third pipeline respectively, and valves are arranged on the first pipeline, the second pipeline and the third pipeline respectively. A vacuum port of the first receiving tank, a vacuum port of the second receiving tank and a vacuum port of the third receiving tank are respectively connected with a vacuum pump.

Description

Technical Field

[0001] This utility model relates to the field of equipment for preparing 5-fluoro-4,6-dichloropyrimidine, and more particularly to an apparatus for preparing 5-fluoro-4,6-dichloropyrimidine. Background Technology

[0002] 5-Fluoro-4,6-dichloropyrimidine is an important chemical intermediate widely used in pharmaceuticals and pesticides. Its preparation process typically involves steps such as reaction formation, mixture separation, and product purification. In existing technologies, the preparation apparatus usually includes a reaction vessel and a receiving tank, where dichloroethane, phosphorus oxychloride, and dihydroxypyrimidine react to produce 5-fluoro-4,6-dichloropyrimidine. These apparatuses have the following shortcomings in separating and purifying the target product: the chlorinating reagent cannot be recovered and reused, making it difficult to reduce costs and increase yield; and the separation process is time-consuming due to the lack of efficient separation equipment. Utility Model Content

[0003] Therefore, there is a need to provide an apparatus for preparing 5-fluoro-4,6-dichloropyrimidine, which solves the problem that dichloroethane and phosphorus oxychloride cannot be recovered and reused in the existing process of preparing 5-fluoro-4,6-dichloropyrimidine.

[0004] To achieve the above objectives, this embodiment provides an apparatus for preparing 5-fluoro-4,6-dichloropyrimidine, comprising a high-level tank, a reaction vessel, a distillation column, a condenser, a vacuum pump, a first receiving tank, a second receiving tank, and a third receiving tank. The inlet of the high-level tank is used to receive dichloroethane and phosphorus oxychloride. The outlet of the high-level tank is connected to the first inlet of the reaction vessel. The reaction vessel is also provided with a feeding port for adding dihydroxypyrimidine. The outlet of the reaction vessel is connected to the inlet of the distillation column. The distillation column is connected to the condenser, which is connected to the vacuum pump. The outlet of the distillation column is connected to the inlets of the first receiving tank, the second receiving tank, and the third receiving tank respectively via a first pipe, a second pipe, and a third pipe. Valves are provided on the first pipe, the second pipe, and the third pipe. The vacuum ports of the first receiving tank, the second receiving tank, and the third receiving tank are respectively connected to the vacuum pump.

[0005] Furthermore, it also includes a sealed feeder, which is located at the feed inlet.

[0006] Furthermore, it also includes a first delivery pump, and the discharge port of the first receiving tank and the discharge port of the second receiving tank are respectively connected to the second inlet of the reactor through a fourth pipe and a fifth pipe, and the first delivery pump is located on the main road formed by the fourth pipe and the fifth pipe.

[0007] Furthermore, it also includes a second conveying pump, and the outlet of the third receiving tank is connected to a sixth pipe, on which the second conveying pump is installed.

[0008] Furthermore, the reactor is equipped with a stirring mechanism.

[0009] Furthermore, the stirring mechanism includes a power source and a stirrer. The power source is located on the top outside of the reaction vessel and is connected to the stirrer, which extends into the reaction vessel.

[0010] Furthermore, the agitator is a paddle agitator or a turbine agitator.

[0011] Furthermore, the reactor is also provided with a discharge port at the center of its bottom.

[0012] Unlike existing technologies, the above technical solution has the following beneficial effects:

[0013] First, in a reaction vessel, dichloroethane, phosphorus oxychloride, and dihydroxypyrimidine react to produce the target compound, 5-fluoro-4,6-dichloropyrimidine, along with other byproducts. Then, the mixture is separated using a distillation column, leveraging the different boiling points of the components for effective separation. A condenser reliquefies the evaporated substances for easy collection. The use of a vacuum pump not only helps maintain a low-pressure environment within the system, which lowers the boiling points of the substances and facilitates separation, but also promotes material flow. Three receiving tanks collect products of different purities or compositions, allowing for further processing or direct use.

[0014] The above description of the utility model is merely an overview of the technical solution of this application. In order to enable those skilled in the art to better understand the technical solution of this application and to implement it based on the description and drawings, and to make the above-mentioned objectives and other objectives, features and advantages of this application easier to understand, the following description is provided in conjunction with the specific embodiments and drawings of this application. Attached Figure Description

[0015] The accompanying drawings are only used to illustrate the principles, implementation methods, applications, features, and effects of specific embodiments of this utility model and other related contents, and should not be considered as limitations on this application.

[0016] Figure 1 This is one of the schematic diagrams of the apparatus for preparing 5-fluoro-4,6-dichloropyrimidine in this embodiment;

[0017] Figure 2 This is the second schematic diagram of the apparatus for preparing 5-fluoro-4,6-dichloropyrimidine in this embodiment;

[0018] Figure 3 This is the third schematic diagram of the apparatus for preparing 5-fluoro-4,6-dichloropyrimidine in this embodiment;

[0019] Figure 4 This is the fourth schematic diagram of the apparatus for preparing 5-fluoro-4,6-dichloropyrimidine in this embodiment;

[0020] Figure 5 This is a schematic diagram of the stirring mechanism in this embodiment.

[0021] Explanation of reference numerals in the attached figures:

[0022] 1. High-level tank;

[0023] 2. Reactor; 21. Discharge port;

[0024] 3. Distillation column;

[0025] 4. Condenser;

[0026] 5. Vacuum pump;

[0027] 6. First receiving tank;

[0028] 7. Second receiving tank;

[0029] 8. Third receiving tank;

[0030] 9. Mixing mechanism; 91. Power source; 92. Agitator;

[0031] 10. Enclosed feeder;

[0032] 110. First Pipeline;

[0033] 120. Second pipeline;

[0034] 130. The third pipeline;

[0035] 140. The fourth pipeline;

[0036] 150. The Fifth Pipeline;

[0037] 160. The Sixth Pipeline;

[0038] 170. First delivery pump;

[0039] 180. Second delivery pump. Detailed Implementation

[0040] To illustrate the possible application scenarios, technical principles, implementable specific solutions, and achievable objectives and effects of this application in detail, the following description, in conjunction with the listed specific embodiments and accompanying drawings, provides a detailed explanation. The embodiments described herein are merely illustrative of the technical solutions of this application and are therefore intended to limit the scope of protection of this application.

[0041] In this document, the term "embodiment" means that a specific feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The term "embodiment" appearing in various places throughout the specification does not necessarily refer to the same embodiment, nor does it specifically limit its independence or connection with other embodiments. In principle, in this application, as long as there are no technical contradictions or conflicts, the technical features mentioned in each embodiment can be combined in any way to form corresponding implementable technical solutions.

[0042] Unless otherwise defined, the technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains; the use of related terms herein is merely for the purpose of describing particular embodiments and is not intended to limit this application.

[0043] In the description of this application, the term "and / or" is used to describe the logical relationship between objects, indicating that three relationships can exist. For example, A and / or B means: A exists, B exists, and A and B exist simultaneously. Additionally, the character " / " in this document generally indicates that the preceding and following objects have an "or" logical relationship.

[0044] In this application, terms such as “first” and “second” are used only to distinguish one entity or operation from another, and do not necessarily require or imply any actual quantity, hierarchy or order relationship between these entities or operations.

[0045] Without further limitations, the use of terms such as “comprising,” “including,” “having,” or other similar open-ended expressions in this application is intended to cover non-exclusive inclusion, which does not exclude the presence of additional elements in a process, method, or product that includes the stated elements, such that a process, method, or product that includes a list of elements may include not only those defined elements but also other elements not expressly listed, or elements inherent to such a process, method, or product.

[0046] Similar to the understanding in the Examination Guidelines, in this application, expressions such as "greater than," "less than," and "exceeding" are understood to exclude the stated number; expressions such as "above," "below," and "within" are understood to include the stated number. Furthermore, in the description of the embodiments in this application, "multiple" means two or more (including two), and similar expressions related to "multiple" are also understood in this way, such as "multiple groups" and "multiple times," unless otherwise explicitly specified.

[0047] In the description of the embodiments of this application, the space-related expressions used, such as "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "vertical," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential," indicate the orientation or positional relationship based on the orientation or positional relationship shown in the specific embodiments or drawings. They are only for the purpose of describing the specific embodiments of this application or for the reader's understanding, and do not indicate or imply that the device or component referred to must have a specific position, a specific orientation, or be constructed or operated in a specific orientation. Therefore, they should not be construed as limitations on the embodiments of this application.

[0048] Unless otherwise expressly specified or limited, the terms "installation," "connection," "linking," "fixing," and "setting," as used in the description of the embodiments of this application, should be interpreted broadly. For example, "connection" can be a fixed connection, a detachable connection, or an integral arrangement; it can be a direct connection or an indirect connection through an intermediate medium; it can be a relationship of two components combined together, an interaction relationship between two components, or a connection within two structures. Those skilled in the art to which this application pertains can understand the specific meaning of the above terms in the embodiments of this application according to the specific circumstances.

[0049] Please see Figures 1 to 5 This embodiment provides an apparatus for preparing 5-fluoro-4,6-dichloropyrimidine, including a high-level tank 1, a reaction vessel 2, a distillation column 3, a condenser 4, a vacuum pump 5, a first receiving tank 6, a second receiving tank 7, and a third receiving tank 8. The inlet of the high-level tank 1 is used to receive dichloroethane and phosphorus oxychloride. The outlet of the high-level tank 1 is connected to the first inlet of the reaction vessel 2. The reaction vessel 2 is also provided with a feeding port for adding dihydroxypyrimidine. The outlet of the reaction vessel 2 is connected to the inlet of the distillation column 3. The distillation column 3 is connected to a condenser 4, which is connected to a vacuum pump 5. The outlet of the distillation column 3 is connected to the inlet of the first receiving tank 6, the inlet of the second receiving tank 7, and the inlet of the third receiving tank 8 through the first pipe 110, the second pipe 120, and the third pipe 130, respectively. Valves are provided on the first pipe 110, the second pipe 120, and the third pipe 130. The vacuum ports of the first receiving tank 6, the second receiving tank 7, and the third receiving tank 8 are connected to the vacuum pump 5, respectively.

[0050] First, in reactor 2, dichloroethane, phosphorus oxychloride, and dihydroxypyrimidine react to form the target compound 5-fluoro-4,6-dichloropyrimidine, along with other byproducts. Then, the mixture is separated using distillation column 3, leveraging the different boiling points of the components for effective separation. Condenser 4 reliquefies the evaporated substances for easy collection. Vacuum pump 5 not only helps maintain a low-pressure environment within the system, which lowers the boiling points of the substances and facilitates separation, but also promotes material flow. Three receiving tanks collect products of different purities or compositions, allowing for further processing or direct use.

[0051] Please see Figure 2 In this embodiment, the apparatus further includes a sealed feeder 10, which is located at the feed inlet. The sealed feeder 10 operates on the principle of maintaining the airtightness of the reaction environment. This sealed feeder 10 is designed to safely add solid reactants (such as dihydroxypyrimidine), ensuring that the entire feeding process takes place in a closed environment, preventing outside air or impurities from entering the reaction system. The sealed feeder 10 is also designed to allow liquids to be added first, followed by solids, which facilitates the dissolution of the solids. Optionally, the sealed feeder 10 typically includes an operable gate or piston structure, allowing the operator to introduce solid materials without disrupting the internal pressure balance of the system. When solid materials need to be added, the operator first closes the valve connected to the reactor 2, then opens the inlet on the sealed feeder 10 and loads the solid materials into it. Afterward, the inlet is closed, and the outlet to the reactor 2 is opened, allowing the solid materials to fall into the reactor 2.

[0052] Please see Figure 1 In this embodiment, the apparatus further includes a first transfer pump 170. A first receiving tank 6 can be used to receive dichloroethane, and a second receiving tank 7 can be used to receive phosphorus oxychloride. The outlet of the first receiving tank 6 and the outlet of the second receiving tank 7 are connected to the second inlet of the reactor 2 via a fourth pipe 140 and a fifth pipe 150, respectively. The first transfer pump 170 is located on the main pipeline formed by the fourth pipe 140 and the fifth pipe 150. The main function of the first transfer pump 170 is to provide the necessary pressure within the apparatus to ensure that dichloroethane and phosphorus oxychloride can be smoothly transferred from the receiving tanks to the reactor 2. When these raw materials need to be replenished, the operator can start the first transfer pump 170, which will pump the materials to the reactor 2 through the fourth pipe 140 and the fifth pipe 150. Since the transfer pump is located on the main pipeline, it can simultaneously or selectively transport both materials, depending on the opening and closing state of the valves. Furthermore, by adjusting the operating parameters of the transfer pump (such as flow rate), the amount of material entering the reactor 2 can be precisely controlled to optimize the reaction conditions.

[0053] Please see Figure 3In this embodiment, the device further includes a second transfer pump 180. A sixth pipe 160 is connected to the outlet of the third receiving tank 8, and the second transfer pump 180 is mounted on the sixth pipe 160. The main function of the second transfer pump 180 is to provide the necessary pressure within the device to ensure that materials can be smoothly transported from the third receiving tank 8 to other equipment or storage areas. When materials in the third receiving tank 8 need to be processed or reused, the operator can start the second transfer pump 180, which will pump the materials to their destination through the sixth pipe 160. Because the transfer pump is located on this pipe, it can independently control the material flow along this path, depending on the specific needs of the system. Furthermore, by adjusting the operating parameters (such as flow rate) of the second transfer pump 180, the amount and speed of material conveyed can be precisely controlled.

[0054] Please see Figure 4 and Figure 5 In this embodiment, the reactor 2 is equipped with a stirring mechanism 9. Stirring can accelerate the diffusion process between liquids, increase the contact area between reactants, thereby improving the mass transfer rate and facilitating a faster and more complete reaction. Effective stirring helps to homogenize the temperature distribution within the reactor 2, preventing localized overheating or uneven cooling, which is particularly important for some temperature-sensitive reactions.

[0055] Please see Figure 4 and Figure 5 In this embodiment, the stirring mechanism 9 includes a power source 91 and a stirrer 92. The power source 91 is located on the top outside of the reactor 2 and is connected to the stirrer 92, which extends into the reactor 2. The power source 91 provides the necessary mechanical energy, which is transmitted to the stirrer 92 through a transmission device, causing the stirrer 92 to rotate and thus stir the materials inside the reactor 2. Placing the power source 91 outside the reactor 2 reduces the safety risks that may arise from direct exposure of electrical equipment to the chemical environment, especially for flammable, explosive, or corrosive materials. The location of the power source 91 outside the reactor 2 facilitates maintenance and replacement without requiring disassembly of the reactor 2, reducing maintenance costs and time.

[0056] Please see Figure 5 In this embodiment, the agitator 92 is a paddle agitator 92, which includes one or more straight or curved blades, typically mounted on a vertical shaft. Alternatively, the agitator 92 is a turbine agitator 92, which consists of multiple inclined small blades forming a turbine-like structure.

[0057] Please see Figure 1In this embodiment, a discharge port 21 is also provided at the center of the bottom of the reactor 2. The discharge port 21 is located at the lowest point of the reactor 2, ensuring that all materials can be completely discharged and avoiding residue. The discharge port 21 is typically equipped with appropriate valves (such as ball valves or butterfly valves) to control the material discharge process and prevent material leakage during non-operational periods. Furthermore, auxiliary equipment may be provided near the discharge port 21, such as a heating jacket (to prevent high-viscosity materials from solidifying) or a purging gas inlet (to clean residues from the pipeline).

[0058] The working principle of the device is explained below:

[0059] Before starting the reaction, ensure that reactor 2 and the sealed feeder 10 are dry, and turn on vacuum pump 5 to maintain a negative pressure environment. Dichloroethane and phosphorus oxychloride are precisely metered and introduced into reactor 2 through high-level tank 1. Then, dihydroxypyrimidine is transferred to the sealed feeder 10 and smoothly added to reactor 2 while maintaining the temperature of reactor 2 at 5-20°C. The design of the sealed feeder 10 ensures the safe addition of solid materials and avoids the introduction of air or other contaminants. After feeding, gradually raise the temperature inside reactor 2 to 75-85°C and maintain this temperature while stirring. During this period, the reactants are thoroughly mixed and undergo a chemical reaction to generate the target product, 5-fluoro-4,6-dichloropyrimidine. The reaction conditions must be strictly monitored throughout the process to ensure the reaction proceeds as expected until the central control system detects compliance. Once the central control system confirms the reaction is complete, slowly increase the temperature to promote the evaporation of unreacted substances and the separation of other byproducts. The crude product is further purified through distillation column 3 to obtain a high-purity finished product. Finally, the crude 5-fluoro-4,6-dichloropyrimidine is transferred to the third receiving tank 8. Solvents and other recyclable materials generated during the reaction are directed to dedicated first and second receiving tanks 6 and 7 for storage. After appropriate processing, these materials can be recycled back into the reaction vessel 2, thus achieving solvent recycling, reducing production costs, and minimizing waste emissions.

[0060] Finally, it should be noted that although the above embodiments have been described in the text and drawings of this application, this should not limit the scope of patent protection of this application. Any technical solutions that are based on the essential concept of this application and utilize the content described in the text and drawings of this application, resulting in equivalent structural or procedural substitutions or modifications, as well as the direct or indirect application of the technical solutions of the above embodiments to other related technical fields, are all included within the scope of patent protection of this application.

Claims

1. An apparatus for preparing 5-fluoro-4,6-dichloropyrimidine, characterized in that, The system includes a high-level tank, a reaction vessel, a distillation column, a condenser, a vacuum pump, a first receiving tank, a second receiving tank, and a third receiving tank. The inlet of the high-level tank is used to receive dichloroethane and phosphorus oxychloride. The outlet of the high-level tank is connected to the first inlet of the reaction vessel. The reaction vessel is also provided with a feed port for adding dihydroxypyrimidine. The outlet of the reaction vessel is connected to the inlet of the distillation column. The distillation column is connected to the condenser, which is connected to the vacuum pump. The outlet of the distillation column is connected to the inlets of the first receiving tank, the second receiving tank, and the third receiving tank via a first pipe, a second pipe, and a third pipe, respectively. Valves are provided on the first pipe, the second pipe, and the third pipe. The vacuum ports of the first receiving tank, the second receiving tank, and the third receiving tank are respectively connected to the vacuum pump.

2. The apparatus according to claim 1, characterized in that, It also includes a sealed feeder, which is located at the feed inlet.

3. The apparatus according to claim 1, characterized in that, It also includes a first delivery pump. The discharge port of the first receiving tank and the discharge port of the second receiving tank are respectively connected to the second inlet of the reactor through a fourth pipe and a fifth pipe. The first delivery pump is located on the main road formed by the fourth pipe and the fifth pipe.

4. The apparatus according to claim 1, characterized in that, It also includes a second conveying pump, and the outlet of the third receiving tank is connected to a sixth pipe, on which the second conveying pump is installed.

5. The apparatus according to claim 1, characterized in that, The reactor is equipped with a stirring mechanism.

6. The apparatus according to claim 5, characterized in that, The stirring mechanism includes a power source and a stirrer. The power source is located on the top outside of the reaction vessel and is connected to the stirrer, which extends into the reaction vessel.

7. The apparatus according to claim 6, characterized in that, The agitator is a paddle agitator or a turbine agitator.

8. The apparatus according to claim 1, characterized in that, The reactor is also equipped with a discharge port at the bottom center.

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