Device for synthesizing florfenicol intermediate (1R, 2R)-p-methylsulfonyl phenyl serinol

Abstract

The utility model provides a florfenicol intermediate (1R, 2R)-p-methylsulfonyl phenyl serinol synthesizer, which comprises a reduction reaction kettle, the top of the reduction reaction kettle is respectively connected with a configuration kettle, a dripping tank, a first feeder, a feeding bin, a water source and an N2 source through pipelines, the water source and the N2 source are further connected to the configuration kettle through pipelines, and the dripping tank is connected with the first feeder through a pipeline. The configuration kettle is connected with a second feeder through a pipeline, and a discharge hole in the bottom of the reduction reaction kettle is sequentially connected with a concentration crystallization kettle and a centrifugal machine. The florfenicol intermediate synthesis device has the beneficial effects that the florfenicol intermediate can be quickly and effectively synthesized, and the production efficiency and the production quality of the florfenicol intermediate are greatly improved.

Description

TECHNICAL FIELD

[0001] The utility model belongs to the fluorobenil intermediate synthesis technical field, especially to a kind of fluorobenil intermediate (1R, 2R)-p-methylsulfone sulfonyl phenylserine alcohol synthesis device. BACKGROUND

[0002] Florfenicol is often used in veterinary clinic to prevent and treat gram-positive, gram-negative and thiamphenicol-resistant bacterial diseases due to its broad antibacterial spectrum, good absorption, extensive distribution in vivo and other characteristics. Therefore, there is a great demand for (1R, 2R)-p-methylsulfone sulfonyl phenylserine alcohol as a fluorobenil intermediate, and high-quality demand. However, the current production of this fluorobenil intermediate often has poor product quality and slow production speed, which affects its production to some extent. UTILITY MODEL CONTENT

[0003] Therefore, the utility model aims to overcome the above-mentioned problems in the prior art, and provides a fluorobenil intermediate (1R, 2R)-p-methylsulfone sulfonyl phenylserine alcohol synthesis device.

[0004] To achieve the above-mentioned purpose, the technical scheme of the utility model is as follows:

[0005] A fluorobenil intermediate (1R, 2R)-p-methylsulfone sulfonyl phenylserine alcohol synthesis device, comprising a reduction reaction kettle, a configuration kettle, a dropping tank, a first feeder and a feeding bin connected to the top of the reduction reaction kettle through pipelines, a water source and an N2 source, the water source and the N2 source are also connected to the configuration kettle through pipelines, and a second feeder is connected to the configuration kettle through a pipeline, and a concentrated crystallization kettle and a centrifuge are connected to the outlet of the bottom of the reduction reaction kettle in sequence.

[0006] Further, the position of the feeding bin is higher than the position of the reduction reaction kettle.

[0007] Further, the reduction reaction kettle comprises a kettle body and a cover body fixed to the opening at the top of the kettle body, a collecting plate is hung and fixed to the upper side inside the kettle body, a through hole is formed in the middle of the collecting plate, a rotating stirring mechanism is arranged inside the kettle body, the stirring mechanism comprises a rotating shaft vertically penetrating through the through hole, a first stirring paddle below the collecting plate and a second stirring paddle above the collecting plate are fixed to the rotating shaft, a gap is provided between the through hole and the rotating shaft, a first inlet, a second inlet, a third inlet, a fourth inlet, a fifth inlet and a sixth inlet are provided on the upper side of the cover body, the first inlet is connected to the configuration kettle, the second inlet is connected to the dropping tank, the third inlet is connected to the first feeder, the fourth inlet is connected to the feeding bin, the fifth inlet is connected to the water source, and the sixth inlet is connected to the N2 source.

[0008] Further, the circumferential inner wall at the upper side of the kettle body is fixed with an L-shaped connecting ridge, the bottom of the collecting plate is concave downward, and the top is provided with an inverted L-shaped lap joint along the circumference outward, which is fixed in the connecting ridge.

[0009] Further, the inner side of the vertical section of the lap joint is fixed with a rubber ring, which is extruded between the lap joint and the connecting ridge.

[0010] Further, the upper side of the lap joint is uniformly provided with a plurality of handles.

[0011] Further, the upper side of the cover body is fixed with a motor, and the output end of the motor is fixed with the rotating rod.

[0012] Further, the first stirring paddle comprises a U-shaped connecting frame and a plurality of connecting rods fixed uniformly in the connecting frame, and the middle of the connecting plate and the bottom of the connecting frame are fixed with the rotating rod.

[0013] Further, the second stirring paddle comprises a connecting cylinder, the bottom of which is fixed with a stirring rod symmetrically, and the upper part of the connecting cylinder is higher than the collecting plate and is fixed with the rotating rod through bolts.

[0014] Further, the bottom of the kettle body is also provided with a sampling port, and a switch valve is arranged on the sampling port.

[0015] Further, the outer side of the kettle body is provided with a jacket.

[0016] Compared with the prior art, the present application has the following advantages:

[0017] (1) The fluorobenilca intermediate (1R, 2R)-p-methylsulfone phenylalaninol synthesis device can quickly and effectively synthesize fluorobenilca intermediate, greatly improving the production efficiency and production quality;

[0018] (2) The reduction reaction kettle is provided with a collecting plate inside, which can preliminarily mix the materials put into the kettle body, and the second stirring paddle is used for stirring in the process, so that the preliminary mixing has a certain uniformity, and then the through hole falls down and the first stirring paddle is used for thorough stirring, which effectively improves the solution mixing and reaction speed. BRIEF DESCRIPTION OF DRAWINGS

[0019] The drawings that form a part of the present application are used to provide a further understanding of the present application, and the illustrative embodiments of the present application and their descriptions are used to explain the present application, and do not constitute an improper limitation on the present application. In the drawings:

[0020] Figure 1 The fluorobenilca intermediate (1R, 2R)-p-methylsulfone phenylalaninol synthesis device structure diagram described in the embodiments of the present application;

[0021] Figure 2 A reduction reaction kettle structure schematic view is described in the embodiments of the present application.

[0022] Figure 3 A second stirring paddle structure schematic view is described in the embodiments of the present application.

[0023] Explanation of reference signs:

[0024] 1, reduction reaction kettle; 11, kettle body; 1101, discharge port; 1102, sampling port; 12, cover body; 13, material collecting plate; 1301, overlapping edge; 1302, handle; 1303, through hole; 14, connecting edge; 15, rotating rod; 16, first stirring paddle; 1601, connecting frame; 1602, connecting rod; 17, second stirring paddle; 1701, connecting cylinder; 1702, stirring rod; 18, jacket; 19, motor; 110, bolt-nut pair; 2, configuration kettle; 3, second feeder; 4, dropping tank; 5, first feeder; 6, feeding bin; 7, concentration crystallization kettle; 8, centrifuge. DETAILED DESCRIPTION

[0025] It should be noted that the embodiments in the present application and the features in the embodiments can be combined with each other without conflict.

[0026] In the description of the present application, it should be understood that the orientation or position relationship indicated by the terms "center", "longitudinal", "transverse", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like is based on the orientation or position relationship shown in the drawings, and is only for the convenience of describing the present application and simplifying the description, and does not indicate or imply that the device or element must have a particular orientation, be constructed and operated in a particular orientation, therefore it cannot be understood as a limitation on the present application. In addition, the terms "first", "second" and the like are only for the purpose of description, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the technical features indicated. Therefore, the features limited by "first", "second" and the like can explicitly or implicitly include one or more of the features. In the description of the present application, unless otherwise specified, the meaning of "a plurality of" is two or more.

[0027] In the description of the utility model, it is necessary to explain, unless another explicit provision and limitation, term "installation", "link", "connection" should do broad sense understanding, for example, can be fixed connection, also can be detachable connection, or integrally connected, can be mechanical connection, also can be electrical connection, can be direct connection, also can be indirectly connected through intermediate medium, can be the intercommunication of two elements. For ordinary skilled in the art, the above-mentioned terms can be understood by the specific meaning in the utility model through specific circumstances.

[0028] The utility model will be described in detail below with reference to the drawings and in combination with the embodiments.

[0029] As shown in the figure, a fluorobenidix intermediate (1R, 2R)-p-methylsulfone phenylalaninol synthesis device, including reduction reaction kettle 1, reduction reaction kettle 1 top is connected with configuration kettle 2, drop tank 4, first feeder 5 and feeding bin 6 respectively through pipeline, and water source and N2 source, water source and N2 source are also connected to configuration kettle 2 through pipeline, and second feeder 3 is connected on configuration kettle 2 through pipeline, and the discharge port 1101 at the bottom of reduction reaction kettle 1 is connected with concentration crystallization kettle 7 and centrifuge 8 in turn.

[0030] The position of feeding bin 6 is higher than the position of reduction reaction kettle 1.

[0031] Reduction reaction kettle 1 includes kettle body 11 and cover 12 fixed at the opening at the top of kettle body 11, the inside of kettle body 11 is hingedly connected with the upper side of the collection plate 13, the middle of collection plate 13 is provided with through hole 1303, the inside of kettle body 11 is provided with rotatable stirring mechanism, stirring mechanism includes vertical through hole 1303 and is provided with first stirring paddle 16 and second stirring paddle 17 below collection plate 13 and above the upper side of collection plate 13, the gap is provided between through hole 1303 and rotating rod 15, the upper side of cover 12 is provided with first inlet, second inlet, third inlet, fourth inlet, fifth inlet, sixth inlet (not shown in the figure), the first inlet is connected with configuration kettle 2, the second inlet is connected with drop tank 4, the third inlet is connected with first feeder 5, the fourth inlet is connected with feeding bin 6, the fifth inlet is connected with water source, and the sixth inlet is connected with N2 source. Figure 2

[0032] The inside of kettle body 11 is hingedly connected with the upper side of the connection along 14 along the circumferential wall, the bottom of collection plate 13 is concave downward, which is convenient for collecting materials, and the top circumferential wall is provided with inverted L-shaped lap joint along 1301, which is lap joint fixed in connection along 14.

[0033] ​The rubber ring (not shown in the figure) is fixed inside the vertical section of the lap joint 1301, and is pressed between the lap joint 1301 and the connecting joint 14, so as to fix the aggregate plate 13 to the connecting joint 14.

[0034] A plurality of handles 1302 are evenly arranged on the upper side of the lap joint 1301, so as to facilitate the disassembly and assembly of the aggregate plate 13 on the connecting joint 14.

[0035] The motor 19 is fixed on the upper side of the cover 12, and the output end of the motor 19 is fixed to the rotating rod 15. The rotating rod 15 is driven to rotate by the motor 19.

[0036] The first stirring paddle 16 comprises a U-shaped connecting frame 1601 and a plurality of connecting rods 1602 fixed to the connecting frame 1601. The middle of the connecting plate and the bottom of the connecting frame 1601 are fixed to the rotating rod 15. In this embodiment, the connecting plate and the bottom of the connecting frame 1601 are welded to the rotating rod 15.

[0037] The second stirring paddle 17 comprises a connecting cylinder 1701, and the stirring rod 1702 is symmetrically fixed to the bottom of the connecting cylinder 1701. The upper part of the connecting cylinder 1701 is higher than the aggregate plate 13 and is fixed to the rotating rod 15 by bolts, so as to avoid the long-term immersion of the bolts in the mixed solution on the aggregate plate 13. In this embodiment, the connecting cylinder 1701 is arranged, so as to facilitate the disassembly and assembly of the second stirring paddle 17, and facilitate the disassembly and assembly of the stirring unit and the aggregate plate 13 in the kettle body 11.

[0038] The sampling port 1102 is arranged at the bottom of the kettle body 11, and a switch valve is arranged on the sampling port 1102, so as to take samples and understand the reaction progress in the kettle body 11 at any time.

[0039] The jacket 18 is arranged on the outer side of the kettle body 11, and the heating coil and the cooling coil arranged in the jacket 18 can heat and cool the kettle body 11.

[0040] In this embodiment, the pH meter, the temperature sensor and the pressure gauge are arranged on the kettle body 11, so as to monitor the internal environment of the kettle body 11.

[0041] In this embodiment, the sealing ring is arranged between the cover 12 and the kettle body 11, and is fixed by a plurality of bolt-nut pairs 110.

[0042] The working process of this embodiment is as follows:

[0043] The water is added to the configuration kettle 2 by the flow meter, and the potassium borohydride is added to the configuration kettle 2 by the second feeder 3, and is dissolved by the stirring unit in the configuration kettle 2.

[0044] The water is added to the reduction reaction kettle 1, the D-ethyl ester is added to the reduction reaction kettle 1 through the high-layer feeding bin 6, the calcium chloride is added to the reduction reaction kettle 1 through the second feeder 5, the N2 is continuously introduced through the N2 source, the potassium borohydride solution is slowly pressed into the reduction reaction kettle 1, the pH value is automatically controlled through the pH meter on the reduction reaction kettle 1, the acid aqueous solution in the dropping tank 4 is added and dropped, and the pH in the reduction reaction kettle 1 is kept as 8±0.5; the reaction process is monitored through sampling at the sampling port 1102 during the reaction; after the reaction is completed, the acid aqueous solution is added and dropped through the dropping tank 4 to quench the reaction. After the reaction is quenched, the solution after the reaction is pressed into the concentration crystallization kettle 7 through the pipeline, the N2 is returned to normal pressure after being concentrated to a certain extent, the methanol is added, and then cooling and crystallization are carried out; finally, the centrifugation and drying are completed in the centrifugal machine 8, and the material is discharged.

[0045] In the reduction reaction kettle 1, after the liquid materials are respectively added from the corresponding feeding ports, the materials first fall on the material collecting plate 13 and are preliminarily mixed under the stirring action of the second stirring paddle 17. Of course, in the process, the materials can also fall from the through hole 1303 without being stirred. When the materials are added more and the falling amount of the through hole 1303 is greater, the materials are effectively stirred by the second stirring paddle 17. The liquid falls from the through hole 1303 to the lower part of the material collecting plate 13. With the materials being added more and more, the mixed liquid continuously falls through the through hole 1303, and the liquid at the lower part of the kettle body 11 is continuously accumulated until the materials are completely added. In the process and after the material adding is completed, the solution is stirred by the first stirring paddle 16, so that the solution is more uniformly and quickly reacted.

[0046] The above merely describes the preferred embodiments of the utility model and is not used to limit the utility model, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the utility model should be included in the protection scope of the utility model.

Claims

1. A device for the synthesis of florfenicol intermediate (1R, 2R)-p- methylsulfonylphenylalaninol, characterized by: The reduction reaction kettle is connected with a configuration kettle, a dropping tank, a first feeder and a feeding bin, a water source and a N2 source through pipelines respectively on the top thereof, the water source and the N2 source are also connected to the configuration kettle through pipelines, and a second feeder is connected to the configuration kettle through a pipeline, and a concentration crystallization kettle and a centrifuge are connected to the outlet of the reduction reaction kettle in sequence.

2. A device for synthesizing florfenicol intermediate (1R, 2R)-p- methylsulfonyl phenylalaninol according to claim 1, characterized by: The position of the feeding bin is higher than that of the reduction reaction kettle.

3. A device for synthesizing florfenicol intermediate (1R, 2R)-p- methylsulfonyl phenylalaninol according to claim 1, characterized by: The reduction reaction kettle comprises a kettle body and a cover body fixed to the top opening of the kettle body, a collecting plate is fixed to the upper side of the interior of the kettle body, a through hole is formed in the middle of the collecting plate, a rotating stirring mechanism is arranged in the interior of the kettle body, the stirring mechanism comprises a rotating shaft vertically arranged through the through hole, a first stirring paddle below the collecting plate and a second stirring paddle above the collecting plate are fixed to the rotating shaft, a gap is arranged between the through hole and the rotating shaft, a first inlet, a second inlet, a third inlet, a fourth inlet, a fifth inlet and a sixth inlet are arranged on the upper side of the cover body, the first inlet is connected to the configuration kettle, the second inlet is connected to the dropping tank, the third inlet is connected to the first feeder, the fourth inlet is connected to the feeding bin, the fifth inlet is connected to the water source, and the sixth inlet is connected to the N2 source.

4. A device for synthesizing florfenicol intermediate (1R, 2R)-p- methylsulfonyl phenylalaninol according to claim 3, characterized by: An L-shaped connecting ridge is fixed to the circumferential inner wall of the upper side of the interior of the kettle body, the bottom of the collecting plate is concave downward, and a reverse L-shaped lap joint ridge is arranged on the top of the collecting plate.

5. A device for synthesizing florfenicol intermediate (1R, 2R)-p- methylsulfonyl phenylalaninol according to claim 4, characterized by: A rubber ring is fixed to the inner side of the vertical section of the lap joint ridge, and the rubber ring is arranged between the lap joint ridge and the connecting ridge.

6. A device for synthesizing florfenicol intermediate (1R, 2R)-p- methylsulfonyl phenylalaninol according to claim 4, characterized by: A plurality of handles are uniformly arranged on the upper side of the lap joint ridge.

7. A device for synthesizing florfenicol intermediate (1R, 2R)-p- methylsulfonyl phenylalaninol according to claim 3, characterized by: A motor is fixed to the upper side of the cover body, and the output end of the motor is fixed to the rotating shaft.

8. A device for synthesizing florfenicol intermediate (1R, 2R)-p- methylsulfonyl phenylalaninol according to claim 3, characterized by: The first stirring paddle comprises a U-shaped connecting frame and a plurality of connecting rods fixed to the connecting frame, and the middle of the connecting plate and the bottom of the connecting frame are fixed to the rotating shaft.

9. A device for synthesizing florfenicol intermediate (1R, 2R)-p- methylsulfonyl phenylalaninol according to claim 3, characterized by: The second stirring paddle comprises a connecting cylinder, stirring rods are fixed to the bottom of the connecting cylinder in a symmetrical manner, and the upper part of the connecting cylinder is higher than the collecting plate and is fixed to the rotating shaft through bolts.

10. A device for synthesizing florfenicol intermediate (1R, 2R)-p- methylsulfonyl phenylalaninol according to claim 3, characterized by: A sampling port is arranged at the bottom of the kettle body, and a switch valve is arranged on the sampling port.

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