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

A technology for ethyl formate and chemical synthesis, 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 achieves the advantages of reducing safety risks, low cost, and improving yield and purity. Effect

Active Publication Date: 2020-08-21
ASYMCHEM LIFE SCI TIANJIN
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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 technology section, the existing synthetic methods of ethyl piperidine-4-carboxylate have the problems of potential safety hazards, high cost, or low yield and purity of the product. In order to solve the above technical problems, the application provides a continuous synthesis method of ethyl piperidine-4-carboxylate, the continuous synthesis method comprises: dispersing the mixture of ethyl pyridine-4-carboxylate and hydrogen to form The gas-liquid mixture containing small droplets of 50nm to 5mm is used as the reaction raw material; the reaction raw material is continuously input into a fixed-bed reactor for catalytic hydrogenation reaction, and piperidine-4-carboxylate ethyl is continuously discharged.

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

Embodiment 1

[0032] Dispersion process: Use the collision convection method to disperse ethyl pyridine-4-carboxylate and hydrogen, the gas-liquid ratio is 1:100, and form small droplets with a particle size of 50nm to 5mm as the reaction raw material.

[0033] Continuous reaction: Pack 5% Ru / C catalyst in the reaction column. Alumina microspheres (1mm) are used at both ends, the mass of the middle catalyst is 28.38g, the filling height is 300mm, the filling diameter is 19.2mm, and the catalyst particle size is 1mm, which is used as a fixed bed reactor.

[0034]The above-mentioned reaction raw materials are continuously fed into the above-mentioned fixed-bed reactor for 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°C, the pressure drop is less than 100.Pa / m, and it runs stably for 50 hours. The conversion rate is 100%, and the product purity is 9...

Embodiment 2

[0036] Dispersion process: Use the collision convection method to disperse ethyl pyridine-4-carboxylate and hydrogen, the gas-liquid ratio is 1:100, and form small droplets with a particle size of 50nm to 5mm as the reaction raw material.

[0037] Continuous reaction: Pack 5% Ru / C catalyst in the reaction column. Alumina microspheres (1mm) are used at both ends, the mass of the middle catalyst is 28.38g, the filling height is 300mm, the filling diameter is 19.2mm, and the catalyst particle size is 1mm, which is used 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 reaction 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 it runs stably for 50 hours. The conversion rate was 87%, and the product purity was 75%. The c...

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Abstract

The invention provides a continuous synthesis method of ethyl piperidine-4-carboxylate. The continuous synthesis method comprises the following steps: dispersing a mixture of ethyl piperidine-4-carboxylate and hydrogen to form a gas-liquid mixture containing small liquid drops with sizes of 50 nm-5 mm, wherein the gas-liquid mixture is used as a reaction raw material; and continuously inputting the reaction raw material into a fixed bed reactor, carrying out a catalytic hydrogenation reaction, and continuously discharging ethyl pyrazine-2-carboxylate. According to the above forced dispersion process, the reaction raw material can be subjected to high-performance mass transfer in the catalytic hydrogenation reaction process, so the sufficient reaction degree of the reaction raw material isimproved, reaction time is shortened, and the yield and purity of the ethyl piperidine-4-carboxylate can be improved. Compared with batch reaction, the continuous synthesis method has the advantages that the amount of the reaction raw material in unit time is small, the occupied area of a reaction device is small, great advantages are realized in the aspects of heat exchange and equipment pressurebearing improvement, equipment investment cost can be greatly reduced, and safety risks caused by use of a large amount of hydrogen is greatly reduced.

Description

technical field [0001] The invention relates to the technical field of synthesis of pharmaceutical chemicals, in particular to a continuous synthesis method of ethyl piperidine-4-carboxylate and its application. Background technique [0002] Ethyl piperidine-4-carboxylate is an important pharmaceutical and pesticide intermediate, which is widely used in sedative drugs and antiarrhythmic drugs. It is also used in drugs such as drugs. This product is also used in Cu or alloy surface treatment liquid, anti-ash material, copolymer of ethylene and alkyl acetate. [0003] There are many existing synthesis methods for ethyl piperidine-4-carboxylate, among which the simpler method is to carry out catalytic reduction reaction with ethyl isonicotinate (ethyl pyridine-4-carboxylate) in a high-pressure reactor , the main method is: (1) Pd / C as catalyst, H 2 Pressure 20Kg / cm 2 , the yield is 99%; (2) NaBH is used in ethanol 4 -RhCl 3 It is directly reduced by reducing agent, the yi...

Claims

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Application Information

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Patent Type & Authority Applications(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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