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Continuous synthetic method and application of piperidine-4-ethyl carboxylate

A technology for the synthesis of ethyl formate, which is applied in the field of pharmaceutical chemical synthesis, can solve the problems of low product purity, high cost, and low product yield, and achieve the goals of reducing safety risks, low cost, and improving yield and purity Effect

Active Publication Date: 2020-11-06
ASYMCHEM LIFE SCI TIANJIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The main purpose of the present invention is to provide a continuous synthesis method of ethyl piperidine-4-carboxylate and its application, to solve the problem of high cost or low product yield in the existing synthetic method of piperidine-4-ethyl carboxylate and the problem of low product purity

Method used

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preparation example Construction

[0018] As described in the background art section, the existing synthesis methods of ethyl piperidine-4-carboxylate have problems of potential safety hazards, high cost or low product yield and low purity. In order to solve the above technical problems, the present application provides a continuous synthesis method of ethyl piperidine-4-carboxylate, the continuous synthesis method comprises: dispersing a mixture of ethyl pyridine-4-carboxylate and hydrogen to form The gas-liquid mixture containing small droplets of 50 nm to 5 mm is used as the reaction raw material; the reaction raw material is continuously input into the fixed bed reactor for catalytic hydrogenation, and the piperidine-4-ethyl carboxylate is continuously discharged.

[0019] In the present application, ethyl pyridine-4-carboxylate and hydrogen are dispersed to form a gas-liquid mixture containing small droplets of 50 nm to 5 mm, and this is used as a raw material for continuous catalytic hydrogenation. Compar...

Embodiment 1

[0032] Dispersion process: The collision convection method was used to disperse ethyl pyridine-4-carboxylate and hydrogen at a gas-liquid ratio of 1:100 to form small droplets with a particle size of 50nm-5mm, which were used as reaction raw materials.

[0033] Continuous reaction: The reaction column was packed with 5% Ru / C catalyst. Both ends are alumina microspheres (1mm), the middle catalyst packing mass is 28.38g, the packing height is 300mm, the packing diameter is 19.2mm, and the catalyst particle size is 1mm, as a fixed bed reactor.

[0034]The above-mentioned reaction raw materials are continuously fed into the above-mentioned fixed-bed reactor to carry out catalytic hydrogenation reaction to obtain ethyl piperidine-4-carboxylate, wherein the volume space velocity is 0.31h -1 , the reaction pressure is 4.0~4.2MPa, the reaction temperature is 160℃, the pressure drop is less than 100.Pa / m, and the stable operation is 50 hours. The conversion rate was 100%, and the prod...

Embodiment 2

[0036] Dispersion process: The collision convection method was used to disperse ethyl pyridine-4-carboxylate and hydrogen at a gas-liquid ratio of 1:100 to form small droplets with a particle size of 50nm-5mm, which were used as reaction raw materials.

[0037] Continuous reaction: The reaction column was packed with 5% Ru / C catalyst. Both ends are alumina microspheres (1mm), the middle catalyst packing mass is 28.38g, the packing height is 300mm, the packing diameter is 19.2mm, and the catalyst particle size is 1mm, as a fixed bed reactor.

[0038] The above-mentioned reaction raw materials are continuously fed into the above-mentioned fixed-bed reactor for catalytic hydrogenation to obtain ethyl piperidine-4-carboxylate, wherein the volume space velocity is 0.32h -1 , the reaction pressure is 4.0-4.2MPa, the reaction temperature is 80°C, the pressure drop is 100Pa / m, and the operation is stable for 50 hours. The conversion rate was 87%, and the product purity was 75%. The ...

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Abstract

The invention provides a continuous synthesis method of piperidine-4-ethyl formate and application thereof. The continuous synthesis method includes: dispersing a mixture of pyridine-4-ethyl formate and hydrogen to form small droplets with a particle size of 50 nm to 5 mm as reaction raw materials; continuously inputting the reaction raw materials into a fixed-bed reactor Catalytic hydrogenation was carried out and ethyl piperidine-4-carboxylate was discharged continuously. The above-mentioned forced dispersion process can enable the reaction raw materials to carry out high-performance mass transfer in the catalytic hydrogenation reaction process, thereby improving the sufficient reaction degree of the reaction raw materials, shortening the reaction time, and improving the yield and purity of ethyl piperidine-4-carboxylate. Compared with batch reaction, the above continuous synthesis method has less reaction raw materials per unit time, and the area of ​​the reaction device is small, and it has great advantages in heat exchange and improvement of equipment pressure, which can greatly It saves equipment investment costs and greatly reduces the safety risks caused by the massive use of hydrogen.

Description

technical field [0001] The invention relates to the technical field of synthesis of pharmaceutical chemicals, in particular to a continuous synthesis method and application of ethyl piperidine-4-carboxylate. Background technique [0002] Ethyl piperidine-4-carboxylate is an important pharmaceutical and pesticide intermediate. It is widely used in sedative drugs and antiarrhythmic drugs. It is in clinical stage neuropeptide Y5 receptor inhibitor and α4β1 integrin inhibitor. It is also used in medicines and other medicines. The product is also used in Cu or alloy surface treatment fluids, anti-ash materials, copolymers of ethylene and alkyl acetate. [0003] There are many synthetic methods for ethyl piperidine-4-carboxylate, wherein a simpler way is to carry out catalytic reduction reaction with ethyl isonicotinate (ethyl pyridine-4-carboxylate) in a high-pressure reactor , the main methods are: (1) Pd / C is the catalyst, H 2 Pressure 20Kg / cm 2 , the yield was 99%; (2) NaB...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/02C07D211/62
CPCC07D211/02C07D211/62
Inventor 洪浩洪亮陶建胡忠张岩左键王波辉戴瑞智王俊强
Owner ASYMCHEM LIFE SCI TIANJIN
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