CN214088354U - Preparation system containing 3-amino-2-formamide pyridine structure compound - Google Patents
Preparation system containing 3-amino-2-formamide pyridine structure compound Download PDFInfo
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- CN214088354U CN214088354U CN202022890362.6U CN202022890362U CN214088354U CN 214088354 U CN214088354 U CN 214088354U CN 202022890362 U CN202022890362 U CN 202022890362U CN 214088354 U CN214088354 U CN 214088354U
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Abstract
The utility model provides a preparation system who contains 3-amino-2-formamide pyridine structure compound, include: the kettle type reaction mechanism comprises a kettle type reactor I and a kettle type reactor II, and the kettle type reactor I is connected with the kettle type reactor II in parallel; the device comprises a tubular reactor, a first kettle reactor and a second kettle reactor are communicated with the tubular reactor, the tubular reactor is also provided with a first input pipeline used for conveying hydrazine hydrate, one end of the tubular reactor is provided with the first input pipeline, and the other end of the tubular reactor is provided with a first output pipeline; the bottom of the concentrated reaction kettle is sequentially communicated with the centrifuge and the waste liquid collecting barrel through pipelines; the condenser is arranged at the upper end of the concentrated reaction kettle through a pipeline, and the lower part of the condenser is communicated through a pipeline storage tank. The utility model has the characteristics of environment-friendly and effectively reduce safe risk, the operation is convenient.
Description
Technical Field
The utility model belongs to the technical field of chemical industry equipment, a preparation system who contains 3-amino-2-formamide pyridine structural compound is related to.
Background
The pyridine compound is one of varieties with wide development and application range in the current heterocyclic compound, has wide application range, relates to medical intermediates, medical products, pesticides, pesticide intermediates, feeds, feed raw materials and other fields, and the 3-amino-2-formamide pyridine derivative is a very important medical intermediate, so the research on the preparation of the 3-amino-2-formamide pyridine derivative has certain significance;
in patents WO2019148036, WO2016193812 and WO2015017407, 5-bromo-2-cyano-3-nitropyridine is reported as a raw material, hydrazine hydrate and ferric trichloride hexahydrate are reacted in an ethanol solvent to obtain 3-amino-5-bromo-pyridine-2-formamide, 80% of hydrazine hydrate is adopted in the process, the risk is high, the equipment requirement is high, and certain safety risk exists in industrial production.
In patent WO2012146659, it is reported that 5-bromo-2-cyano-3-nitropyridine is used as a raw material, and 3-amino-5-bromo-pyridine-2-carboxamide is obtained by hydrogenation, wherein expensive raney nickel is used as a catalyst in the process, and high-pressure hydrogenation has high requirements on equipment, and is not suitable for industrial production.
Patent WO2010007114 reports that 5-bromo-2-cyano-3-nitropyridine is used as a raw material, stannous dichloride is used for reduction of nitro groups and hydrolysis of cyano groups to obtain 3-amino-5-bromo-pyridine-2-formamide, and the process uses 4.0 equivalent of stannic chloride, so that the post-treatment is difficult and the process is not suitable for industrial production.
The synthetic routes of the prior art therefore have the following disadvantages: the operation process is complex and there is a safety risk in the preparation process.
In conclusion, in order to solve the defects in the prior art, the utility model designs a preparation system containing 3-amino-2-formamide pyridine structure compound, which is environment-friendly, can improve the yield, effectively reduce the safety risk and is convenient to operate.
Disclosure of Invention
The utility model provides a preparation system containing 3-amino-2-formamide pyridine structure compound, which is used for solving the problems in the prior art, has the advantages of high yield, environmental friendliness, effective reduction of safety risk and convenient operation.
The purpose of the utility model can be realized by the following technical proposal:
a system for preparing a compound having a pyridine structure of 3-amino-2-carboxamide, comprising:
the kettle type reaction mechanism comprises a kettle type reactor I and a kettle type reactor II, and the kettle type reactor I is connected with the kettle type reactor II in parallel;
the device comprises a tubular reactor, a first kettle reactor and a second kettle reactor are communicated with the tubular reactor, the tubular reactor is also provided with a first input pipeline used for conveying hydrazine hydrate, one end of the tubular reactor is provided with the first input pipeline, and the other end of the tubular reactor is provided with a first output pipeline;
the bottom of the concentrated reaction kettle is sequentially communicated with the centrifuge and the waste liquid collecting barrel through pipelines;
the condenser is arranged at the upper end of the concentrated reaction kettle through a pipeline, and the lower part of the condenser is communicated through a pipeline storage tank.
As a further improvement of the scheme, the first kettle reactor is communicated with the tubular reactor through an output pipe of the first kettle reactor.
As a further improvement of the scheme, the two kettle type reactors are communicated with the tubular reactor through the output pipes of the two kettle type reactors.
As a further improvement of the scheme, a metering pump is arranged on an output pipe of the kettle type reactor.
As a further improvement of the scheme, a metering pump is arranged on the second output pipe of the kettle type reactor.
As a further improvement of the scheme, a double-cone dryer is arranged on one side of the centrifugal machine.
As a further improvement of the scheme, the inner diameter of the tubular reactor is 0.5-60 mm.
As a further improvement of the scheme, the length of the tubular reactor is 2-15 m.
Compared with the prior art, the utility model has the advantages that the structural design is reasonable, the preparation method of the compound containing the 3-amino-2-formamide pyridine structure is improved in a breakthrough manner, the microchannel reactor equipment is used for the first time, environment-friendly water is used as a solvent, the safety risk in the use process of hydrazine hydrate is reduced, the yield and the purity of the product are improved, the adaptability of the substrate is wide, the production process has no amplification effect, multiple amplification can be realized through multistage parallel connection, the characteristics of good continuous reaction stability are realized, the operation is simple and convenient, the production period is simple, the pollution is low, the energy consumption is low, and the preparation method is suitable for industrial production; the molar yield is more than 95 percent, compared with the traditional process, the yield of the invention is improved by about 10 percent, the HPLC content of the crude product reaches 97 percent, the production cost is reduced, and the method is safe, reliable, simple and convenient to operate and suitable for large-scale industrial production; the substrate has wide applicability and is suitable for various compounds containing 3-amino-2-formamide pyridine structure; the synthesis of the compound containing the 3-amino-2-formamide pyridine structure is carried out by using the microchannel reactor for the first time, the micro-reactor has good heat transfer effect and strong mixing uniformity, the reaction time is effectively shortened, and the reaction time is shortened to 1-5 minutes from 8-10 hours of the traditional kettle type intermittent reaction; on the basis of improving the reaction conversion rate, the reaction safety risk is further reduced.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
In the figure, the position of the upper end of the main shaft,
10-a first kettle reactor, 11-a second kettle reactor, 12-a first kettle reactor output pipe; 13-an output pipe of the second kettle reactor;
20-tubular reactor, 21-input pipeline I, 22-output pipeline I;
30-a concentrated reaction kettle;
40-centrifugal machine, 41-double cone drier;
50-a waste liquid collecting barrel;
60-a condenser;
70-a storage tank;
80-metering pump.
Detailed Description
The technical solution of the present invention will be further explained with reference to the following embodiments and accompanying drawings.
As shown in the figure, the first and second,
the preparation system of the compound containing the 3-amino-2-formamide pyridine structure comprises the following steps:
the kettle type reaction mechanism comprises a first kettle type reactor 10 and a second kettle type reactor 11, and the first kettle type reactor 10 is connected with the second kettle type reactor 11 in parallel;
the device comprises a tubular reactor 20, a first kettle reactor 10 and a second kettle reactor 11 are communicated with the tubular reactor 20, the tubular reactor 20 is also provided with a first input pipeline 21, the first input pipeline 21 is used for conveying hydrazine hydrate, one end of the tubular reactor 20 is provided with the first input pipeline 21, and the other end of the tubular reactor 20 is provided with a first output pipeline 22;
the concentrated reaction kettle 30 is communicated with the tubular reactor 20 through a first output pipeline 22, and the bottom of the concentrated reaction kettle 30 is sequentially communicated with a centrifugal machine 40 and a waste liquid collecting barrel 50 through pipelines;
the condenser 60 is provided at the upper end of the concentrated reactor 30 through a pipe, and the lower portion of the condenser 60 is communicated with the storage tank 70 through a pipe.
As a further preferred embodiment, the tank reactor I10 is connected to the tubular reactor 20 via a tank reactor I outlet conduit 12.
As a further preferred embodiment, the second tank reactor 11 is communicated with the tubular reactor 20 through a second tank reactor output pipe 13.
As a further preferred embodiment, the output line 12 of the tank reactor is provided with a metering pump 80.
As a further preferred embodiment, a metering pump 80 is arranged on the second output pipe 13 of the tank reactor.
As a further preferred embodiment, a double cone dryer 41 is further provided at one side of the centrifuge 40.
The synthetic routes of the prior art have the following disadvantages: the operation process is complex and there is a safety risk in the preparation process.
In conclusion, in order to solve the defects in the prior art, the utility model designs a preparation system containing 3-amino-2-formamide pyridine structure compound, which is environment-friendly, can improve the yield, effectively reduce the safety risk and is convenient to operate.
Therefore, the utility model designs a preparation system containing 3-amino-2-formamide pyridine structure compound, uses the tubular reactor 20, namely the microchannel reactor carries out the synthesis containing 3-amino-2-formamide pyridine structure compound, the micro-reactor has good heat transfer effect and strong mixing uniformity, effectively shortens the reaction time, and shortens the reaction time to 1-5 minutes from 8-10 hours of the traditional kettle type intermittent reaction; on the basis of improving the reaction conversion rate, the reaction safety risk is further reduced.
The specific operation process is as follows:
8.0kg (0.035mol, 1.0eq) of 5-bromo-2-cyano-3-nitropyridine are weighed out and dissolved in 40.0kg of methanol in a first tank reactor 10, 1.14kg of ferric chloride hexahydrate is weighed, dissolved in 40kg (0.004mol,0.12eq) of process water in a second kettle-type reactor 11, respectively pumped into a mixer through a calibrated metering pump 80, the sample injection speed of the 5-bromine-2-cyano-3-nitropyridine methanol solution is 24.0ml/min, the sample injection speed of the ferric trichloride hexahydrate solution is 20.6ml/min, after being uniformly mixed, the mixture is pumped into a tubular reactor 20 at the speed of 3.0ml/min, namely, a microchannel reactor, and simultaneously pumping 3.52kg of 80% hydrazine hydrate (0.07mol, 2.0eq) solution into the microchannel reactor through a metering pump 80 with a calibrated input pipeline I21 respectively, wherein the injection speed of the 80% hydrazine hydrate solution is 1.71 ml/min. The reaction liquid enters a micro reactor with the channel size of 10mm, the total length of 6m and the inner layer of polytetrafluoroethylene, namely a tubular reactor 20 at the speed of 3.0m/min, the temperature of the reactor is controlled to be 35-45 ℃, and the reaction residence time is 120 s. Collecting effluent liquid at the outlet of the microchannel reactor, concentrating the effluent liquid in a concentration type reaction kettle 30 until no fraction is produced, adding 900g of process water, stirring and separating materials, and performing suction filtration through a centrifuge 40 to obtain light yellow solid with the yield of 95% and the purity of 97.5%. The filter residue forms a filter cake, which is collected and dried by a double cone dryer 41. The waste liquid is collected by the waste liquid collecting barrel 50
Compound 1.1 nuclear magnetic data are as follows:
1H NMR(500MHz,Chloroform-d)δ8.44(d,J＝1.3Hz,1H),7.66(d,J＝1.2Hz,1H),6.70(s,2H),3.50(s,2H).
[ M + H ] molecular ion peak 216.04.
The preferred embodiments of the present invention are described herein, but the scope of the present invention is not limited thereto. Modifications or additions to or replacement by similar means to those skilled in the art to which the invention pertains to the specific embodiments described herein are intended to be covered by the scope of the invention.
Claims (8)
1. A system for preparing a compound containing a pyridine structure of 3-amino-2-carboxamide, comprising:
the kettle type reaction mechanism comprises a first kettle type reactor (10) and a second kettle type reactor (11), and the first kettle type reactor (10) is connected with the second kettle type reactor (11) in parallel;
the device comprises a tubular reactor (20), a first kettle reactor (10) and a second kettle reactor (11) are communicated with the tubular reactor (20), the tubular reactor (20) is also provided with a first input pipeline (21), the first input pipeline (21) is used for conveying hydrazine hydrate, one end of the tubular reactor (20) is provided with the first input pipeline (21), and the other end of the tubular reactor (20) is provided with a first output pipeline (22);
the device comprises a concentrated reaction kettle (30), wherein the concentrated reaction kettle (30) is communicated with a tubular reactor (20) through a first output pipeline (22), and the bottom of the concentrated reaction kettle (30) is sequentially communicated with a centrifugal machine (40) and a waste liquid collecting barrel (50) through a pipeline;
and the condenser (60) is arranged at the upper end of the concentration type reaction kettle (30) through a pipeline, and the lower part of the condenser (60) is communicated with the storage tank (70) through a pipeline.
2. The system for preparing a compound containing a pyridine structure of 3-amino-2-carboxamide according to claim 1, characterized in that the tank reactor one (10) is connected to the tubular reactor (20) via a tank reactor one output line (12).
3. The system for preparing a compound containing a 3-amino-2-carboxamide pyridine structure as claimed in claim 1, characterized in that the second tank reactor (11) is connected to the tubular reactor (20) via a second tank reactor outlet line (13).
4. The system for preparing a compound containing a pyridine structure of 3-amino-2-carboxamide according to claim 1, characterized in that the metering pump (80) is provided on an output pipe (12) of the tank reactor.
5. The system for preparing a compound containing a pyridine structure of 3-amino-2-carboxamide according to claim 1, characterized in that the second outlet pipe (13) of the tank reactor is provided with a metering pump (80).
6. The system for preparing a compound containing a pyridine structure of 3-amino-2-carboxamide according to claim 1, characterized in that the centrifuge (40) is provided with a double-cone drier (41) on one side.
7. The system for preparing a compound containing a 3-amino-2-carboxamide pyridine structure as claimed in claim 1, characterized in that the internal diameter of the tubular reactor (20) is 0.5 to 60 mm.
8. The system for preparing a compound containing a 3-amino-2-carboxamide pyridine structure as claimed in claim 1, characterized in that the length of the tubular reactor (20) is 2 to 15 meters.
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