Synthesizer for m-nitrophenylacetylene

Abstract

The utility model discloses a synthesizer for preparing m-nitrophenylacetylene by taking m-nitrobenzaldehyde as a raw material, which is characterized in that the bottom of a reaction kettle is also provided with a first discharge port, and the first discharge port is also connected with a second feed port of a filter centrifuge through a first transfer pump; a second discharge hole of the filtering centrifugal machine is connected with a filtrate inlet formed in the top of the reaction kettle through a second transfer pump; a first ventilation connector and a second ventilation connector are arranged at the top of the reaction kettle, and a ventilation valve on the first ventilation connector is a three-way ventilation valve. According to the synthesis device disclosed by the utility model, circulating filtration can be carried out in time after reaction of m-nitrobenzaldehyde and dimethyl (1-diazo-2-oxo-propanol)-phosphonate is finished, so that after anhydrous carbonate particles are filtered, an organic solvent is removed by distillation under reduced pressure in time, and a required m-nitrophenylacetylene solution can be post-treated earlier. Therefore, the problems that the product flows through a long pipeline and the consumed time is long are solved.

Description

Technical Field

[0001] This utility model belongs to the field of chemical equipment technology, and relates to m-nitrophenylacetylene, specifically to a synthesis apparatus for m-nitrophenylacetylene. Background Technology

[0002] m-Nitrophenylacetylene, also known as 3-nitrophenylacetylene or 1-ethynyl-3-nitrobenzene, contains two functional groups: nitro and ethynyl. The structural formula of m-nitrophenylacetylene is:

[0003] m-Nitrophenylacetylene is an important intermediate in organic synthesis with wide applications. It can be used to prepare phenylacetylene compounds, such as aromatic aldehydes and ketones. It can also be used to synthesize organic compounds containing nitro substituent groups, such as nitrophenylacetyl alcohols and nitrophenylacetyl acids. Furthermore, it has broad application prospects in pharmaceutical synthesis and dye synthesis. Aminophenylacetylene is an important intermediate in the preparation of polymer materials and a crucial raw material for the synthesis of erlotinib hydrochloride, a quinazoline drug considered one of the most effective anticancer drugs.

[0004] The production of m-nitrobenzeneacetylene uses m-nitrobenzaldehyde as a raw material, which reacts with dimethyl (1-diazo-2-oxo-propanol)-phosphonate in an organic solvent under strongly alkaline conditions of anhydrous carbonate via a Seyferth–Gilbert carbonation reaction. The entire reaction process is simple, efficient, and the reaction conditions are mild. However, the production equipment currently used to perform this reaction is not yet mature and complete in terms of function and performance, and there is an urgent need to upgrade to more systematic and high-performance production equipment. Summary of the Invention

[0005] In view of the shortcomings of the existing technology, the purpose of this utility model is to provide a synthesis device for meta-nitrophenylacetylene, so as to solve the technical problem that the convenience of the synthesis device in the existing technology needs to be further improved.

[0006] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:

[0007] A synthetic apparatus for preparing m-nitrobenzaldehyde as a raw material includes a reactor, a first inlet at the top of the reactor, and a first outlet at the bottom of the reactor. The first outlet is connected to a post-processing pipeline via a first transfer pump.

[0008] The first discharge port is also connected to the second inlet of the filter centrifuge via a first transfer pump; the second discharge port of the filter centrifuge is connected to the filtrate inlet located at the top of the reactor via a second transfer pump.

[0009] The top of the reactor is equipped with a first vent and a second vent, and the vent valve on the first vent is a three-way vent valve.

[0010] This utility model also has the following technical features:

[0011] The reactor is equipped with a stirring shaft, on which a stirring paddle is mounted, and the stirring shaft is driven by a stirring motor.

[0012] The reactor is provided with a solvent outlet at the top, which is connected to the shell-side inlet of the condenser. The shell-side liquid outlet of the condenser recovers the evaporated organic solvent.

[0013] The outer wall of the reactor is provided with a heating jacket, and the outer wall of the reactor inside the heating jacket is provided with a cooling coil.

[0014] The reactor is also equipped with a thermometer and a pressure / vacuum gauge.

[0015] Compared with the prior art, the present invention has the following beneficial technical effects:

[0016] (I) The synthesis apparatus of this invention can promptly circulate and filter after the reaction of m-nitrobenzaldehyde and (1-diazo-2-oxo-propanol)-phosphonate dimethyl ester is completed. This allows for the timely removal of organic solvents by vacuum distillation after the filtration of anhydrous carbonate particles, enabling the required m-nitrobenzyl acetylene solution to undergo post-processing earlier. This solves the problem of long product flow pipelines and long processing time.

[0017] (II) In the synthesis apparatus of this invention, the reaction between m-nitrobenzaldehyde and (1-diazo-2-oxo-propanol)-phosphonate dimethyl ester uses high-quality m-nitrobenzaldehyde and (1-diazo-2-oxo-propanol)-phosphonate dimethyl ester to rapidly synthesize m-nitrobenzyl acetylene, which not only greatly improves the reaction rate, but also controls the product quality from the source, making the product particle size more uniform and significantly improving the product stability. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the overall structure of the synthesis apparatus for meta-nitrophenylacetylene.

[0019] The labels in the diagram represent the following: 1-Reaction vessel, 2-First feed inlet, 3-First discharge outlet, 4-First transfer pump, 5-Post-treatment pipeline, 6-Filter centrifuge, 7-Second feed inlet, 8-Second discharge outlet, 9-Second transfer pump, 10-Filtrate inlet, 11-First vent connector, 12-Second vent connector, 13-Agitator shaft, 14-Agitator paddle, 15-Agitator motor, 16-Solvent outlet, 17-Condenser, 18-Heating jacket, 19-Cooling coil, 20-Thermometer, 21-Pressure / vacuum gauge, 22-Three-way vent valve, 23-Pipeline, 24-Valve.

[0020] The specific content of this utility model will be further explained in detail below with reference to the embodiments. Detailed Implementation

[0021] It should be noted that, unless otherwise specified, all components, equipment and raw materials in this utility model are based on components, equipment and raw materials known in the prior art.

[0022] In this invention, the various devices are mainly connected by pipes 23. Each pipe 23 is equipped with a valve 24 as needed, which is opened or closed according to process requirements. All valves 24 in this invention are commonly used valves in the prior art.

[0023] Following the above technical solution, the following are specific embodiments of this utility model. It should be noted that this utility model is not limited to the following specific embodiments, and all equivalent modifications made based on the technical solution of this application fall within the protection scope of this utility model.

[0024] Example:

[0025] This embodiment provides a synthetic apparatus for preparing m-nitrobenzylene using m-nitrobenzylaldehyde as a raw material, such as... Figure 1 As shown, the reactor includes a reactor 1, with a first feed inlet 2 at the top and a first discharge outlet 3 at the bottom. The first discharge outlet 3 is connected to a post-processing pipeline 5 via a first transfer pump 4.

[0026] like Figure 1 As shown, the first discharge port 3 is also connected to the second inlet port 7 of the filter centrifuge 6 via the first transfer pump 4; the second discharge port 8 of the filter centrifuge 6 is connected to the filtrate inlet 10 provided at the top of the reactor 1 via the second transfer pump 9.

[0027] like Figure 1 As shown, the top of the reactor 1 is provided with a first venting connector 11 and a second venting connector 12, and the venting valve on the first venting connector 11 is a three-way venting valve 22.

[0028] In this embodiment, the reactor 1 is an acid and alkali resistant enamel-lined reactor. The inner wall is lined with an anti-corrosion layer. Reactor 1 can be used for solution reactions and for removing organic solvents by vacuum distillation after filtration.

[0029] In this embodiment, the filter centrifuge 6 can have a circulation path to ensure that fine particles in the solution circulate through the filter centrifuge 6, which can make the removal of fine particles in the solution more complete.

[0030] In this embodiment, the post-processing pipe 5 is connected to a post-processing procedure known in the art.

[0031] In this embodiment, the three-way vent valve 22 can connect to the nitrogen gas and vacuum pump. The first vent connector 16 can be connected to a nitrogen cylinder or a vacuum filter used to provide the reaction environment and reduced pressure environment.

[0032] As a preferred embodiment of this invention, such as Figure 1 As shown, a stirring shaft 13 is installed inside the reactor 1, and a stirring paddle 14 is mounted on the stirring shaft 13. The stirring shaft 13 is driven by a stirring motor 15. In this embodiment, the stirring paddle 14 is a polytetrafluoroethylene multilayer turbine stirring paddle.

[0033] As a preferred embodiment of this invention, such as Figure 1 As shown, the top of the reactor 1 is provided with a solvent outlet 16, which is connected to the shell-side inlet of the condenser 17. The shell-side liquid outlet of the condenser 17 recovers the evaporated organic solvent.

[0034] As a preferred embodiment of this invention, such as Figure 1 As shown, a heating jacket 18 is provided on the outer wall of the reactor 1, and a cooling coil 19 is provided on the outer wall of the reactor 1 inside the heating jacket 18. In this embodiment, a vacuum insulation pipeline covers the outer layer of the heating jacket 18.

[0035] As a preferred embodiment of this invention, such as Figure 1 As shown, a thermometer 20 and a pressure / vacuum gauge 21 are also installed on the reactor 1. The thermometer 20 is used to detect the temperature inside the reactor 1, and its lower end extends into the reactor 1 to a depth of 2 / 3. The pressure / vacuum gauge 21 is used to display the pressure inside the reactor 1 in real time when nitrogen is introduced into the reaction and when the organic solvent is removed by vacuum distillation.

[0036] In this embodiment, the specific working process of the device is illustrated by taking the reaction of m-nitrobenzaldehyde dissolved in anhydrous methanol with anhydrous potassium carbonate and Bestmann-Ohira reagent (i.e., dimethyl (1-diazo-2-oxo-propanol)-phosphonate) as an example:

[0037] Add 5 kg of m-nitrobenzaldehyde, 10 kg of anhydrous potassium carbonate, and 8 kg of Bestmann-Ohira reagent, along with 90 L of anhydrous methanol, in portions through the first inlet 2. Connect the three-way vent valve 22 on the first vent connector 11 to a nitrogen cylinder and introduce nitrogen gas to create a nitrogen atmosphere in the reaction system. Turn on the stirring motor 15 to start stirring with the stirring paddle 14. Heat the mixture to 40°C using the heating jacket 18 and allow it to react for a total of 12 hours. After the reaction is complete, pump the mixed solution through the first transfer pump 4 into the centrifuge 6 and collect the filtrate in the reaction vessel 1. Connect the three-way vent valve 22 on the first vent connector 11 to a vacuum filter to remove the anhydrous methanol under reduced pressure. Recover the anhydrous methanol at the shell-side outlet of the condenser 17.

Claims

1. A m-nitrophenyl acetylene synthesis device, comprising a reaction kettle (1), a first feed inlet (2) is arranged at the top of the reaction kettle (1), a first discharge port (3) is further arranged at the bottom of the reaction kettle (1), the first discharge port (3) is connected with a post-treatment pipeline (5) through a first material transfer pump (4); characterized in that: the first discharge port (3) is further connected with a second feed inlet (7) of a filter centrifuge (6) through the first material transfer pump (4); a second discharge port (8) of the filter centrifuge (6) is connected with a filter liquid inlet (10) arranged at the top of the reaction kettle (1) through a second material transfer pump (9); a first vent connector (11) and a second vent connector (12) are arranged at the top of the reaction kettle (1), a three-way vent valve (22) is arranged on the first vent connector (11).

2. The apparatus for synthesizing m-nitrophenylacetylene according to claim 1, wherein a stirring shaft (13) is arranged in the reaction kettle (1), a stirring paddle (14) is arranged on the stirring shaft (13), and the stirring shaft (13) is driven by a stirring motor (15).

3. The apparatus for synthesizing m-nitrophenylacetylene according to claim 1, wherein a solvent gas outlet (16) is arranged at the top of the reaction kettle (1), the solvent gas outlet (16) is connected with a shell inlet of a condenser (17), and a shell outlet of the condenser (17) recovers evaporated organic solvent.

4. The apparatus for synthesizing m-nitrophenylacetylene according to claim 1, wherein a heating jacket (18) is arranged on the outer wall of the reaction kettle (1), and a cooling coil (19) is arranged on the outer wall of the reaction kettle (1) in the heating jacket (18).

5. The apparatus for synthesizing m-nitrophenylacetylene according to claim 1, wherein a thermometer (20) and a pressure vacuum gauge (21) are further arranged on the reaction kettle (1).

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