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Synthesis method of intermediate 4-piperidone

A synthesis method and technology of piperidone are applied in the field of synthesis of intermediate 4-piperidone to achieve the effects of reducing the generation of by-products, simple operation and good economic benefits

Inactive Publication Date: 2019-11-22
陈建江
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above methods have achieved certain research results, they still have some shortcomings. Therefore, it is of great research significance to develop a more efficient and convenient preparation method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A kind of synthetic method of intermediate 4-piperidone, comprises the following steps:

[0024] (1) Add β-alanine methyl ester to ethanol, place it in a reaction kettle, add ethylene, mix well, cool down to 0°C, add PS-AlCl 3 -SbCl 5 and sodium ethylate, stirred and reacted, after the reaction was completed, cooled to room temperature, and removed ethanol by distillation under reduced pressure;

[0025] (2) Add DMF to the reaction kettle, stir and mix evenly, heat to 110°C, and carry out reflux reaction under stirring condition, after reacting for 1 hour, cool down to room temperature, extract with ethyl acetate, evaporate ethyl acetate, and then reduce pressure distillation to obtain the 4-piperidone.

[0026] PS-AlCl 3 -SbCl 5 The preparation method is, including the following steps: adding polystyrene powder into carbon tetrachloride, heating to 80 ° C, adding AlCl 3 and SbCl 5 , carry out the reflux reaction under stirring conditions, after the reaction is co...

Embodiment 2

[0030] A kind of synthetic method of intermediate 4-piperidone, comprises the following steps:

[0031] (1) Add β-alanine methyl ester to ethanol, place it in a reaction kettle, add ethylene, mix well, cool down to 10°C, add PS-AlCl 3 -SbCl 5 and sodium ethylate, stirred and reacted, after the reaction was completed, cooled to room temperature, and removed ethanol by distillation under reduced pressure;

[0032] (2) Add DMF to the reaction kettle, stir and mix evenly, heat to 130°C, and carry out reflux reaction under stirring conditions, after reacting for 2 hours, cool down to room temperature, extract with ethyl acetate, evaporate ethyl acetate, and then reduce pressure distillation to obtain the 4-piperidone.

[0033] PS-AlCl 3 -SbCl 5 The preparation method is as described in Example 1.

[0034] The molar volume ratio of the usage amount of β-alanine methyl ester and ethanol is 1.5mol / L; the usage molar ratio of β-alanine methyl ester and ethylene is 1:1.4; The mass...

Embodiment 3

[0037] A kind of synthetic method of intermediate 4-piperidone, comprises the following steps:

[0038] (1) Add β-alanine methyl ester to ethanol, place it in a reaction kettle, add ethylene, mix well, cool down to 0°C, add PS-AlCl 3 -SbCl 5 and sodium ethylate, stirred and reacted, after the reaction was completed, cooled to room temperature, and removed ethanol by distillation under reduced pressure;

[0039] (2) Add DMF to the reaction kettle, stir and mix evenly, heat to 130°C, and carry out reflux reaction under stirring condition, after reacting for 1 hour, cool down to room temperature, extract with ethyl acetate, evaporate ethyl acetate, and then reduce pressure distillation to obtain the 4-piperidone.

[0040] PS-AlCl 3 -SbCl 5 The preparation method is as described in Example 1.

[0041] The molar volume ratio of the usage amount of β-alanine methyl ester and ethanol is 1.5mol / L; the usage molar ratio of β-alanine methyl ester and ethylene is 1:1.2; The mass ra...

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PUM

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Abstract

The invention discloses a synthesis method of an intermediate 4-piperidone. The method comprises the following steps: adding beta-alanine methyl ester into ethanol, placing the raw material into a reaction kettle, adding ethylene, uniformly mixing the raw materials, cooling the raw materials to 0-10 DEG C, adding a catalyst aid and sodium ethoxide, stirring the raw materials for reaction, and cooling a reaction product to room temperature after the reaction is finished; and performing reduced pressure distillation to remove ethanol; adding DMF into a reaction kettle, uniformly stirring and mixing the components, heating the mixture to 110-130 DEG C, and carrying out reflux reaction under a stirring condition for 1-2 hours; cooling the reaction product to room temperature, extracting the reaction product with ethyl acetate, performing evaporation to remove ethyl acetate, and carrying out reduced pressure distillation to obtain the 4-piperidone. The synthesis method disclosed by the invention adopts a one-pot method, does not need an intermediate purification step, reduces resource waste, is simple to operate, short in production process, high in raw material conversion rate and relatively low in production cost, and has relatively high economic benefits.

Description

technical field [0001] The invention relates to the field of pharmaceutical intermediates, in particular to a method for synthesizing the intermediate 4-piperidone. Background technique [0002] Heterocyclic compounds are the most important class of chemical substances, widely distributed in nature, and widely used in medicine, pesticides, dyes, and fine chemicals. Piperidine, also known as hexahydropyridine, is an important new heterocyclic organic intermediate. Piperidine derivatives are widely used in the fields of synthetic medicine, pesticides and rubber additives. [0003] In the rubber additives industry, it can be used to synthesize thiuram super vulcanization accelerators, which are non-polluting and non-discoloring, and are suitable for light-colored rubber and food-contact products; they can also be used to synthesize dithio Carbamate accelerators, which are suitable for latex products. Among them, in the field of medicine, piperidine compounds are widely used i...

Claims

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Application Information

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IPC IPC(8): C07D211/74B01J31/26
CPCB01J31/26C07D211/74
Inventor 陈建江
Owner 陈建江