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Reduction preparation method of 4-(trifluoromethyl)piperidine

A technology for trifluoromethylpiperidine and trifluoromethylpyridine is applied in the field of reduction preparation for preparing 4-trifluoromethylpiperidine and 4-trifluoromethylpiperidine, and can solve the problems of expensive raw materials, complicated processes, problems such as low output, to achieve the effects of convenient preparation, simple process, and easy availability of raw materials

Inactive Publication Date: 2012-07-11
SHANGHAI SINOFLUORO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the above problems, the present invention overcomes the problems of relatively expensive raw materials, complicated process and low output, and provides a method for reducing and preparing 4-trifluoromethylpyridine

Method used

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  • Reduction preparation method of 4-(trifluoromethyl)piperidine
  • Reduction preparation method of 4-(trifluoromethyl)piperidine
  • Reduction preparation method of 4-(trifluoromethyl)piperidine

Examples

Experimental program
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Effect test

Embodiment 1

[0022] A reduction preparation method of 4-trifluoromethylpiperidine, comprising the following steps:

[0023] (1) Preparation of 4-trifluoromethylpiperidine:

[0024] At room temperature, 4-trifluoromethylpyridine and palladium-carbon are put into the reactor, and the amount of palladium-carbon catalyst is 2% of the 4-trifluoromethylpyridine weight, and hydrogen is passed into the reactor and kept for 3 ~12 atmospheric pressure, carry out hydrogenation under stirring, carry out hydrogenation reduction reaction under the catalysis of palladium carbon, generate 4-trifluoromethylpiperidine, reaction is shown in formula 2:

[0025]

[0026]

[0027] Formula 2

[0028] (2) Purification of 4-trifluoromethylpiperidine:

[0029] The reaction mixture in the step (1) is filtered to remove the catalyst, and the obtained filtrate is concentrated by distillation to remove ethanol. The temperature of the distillation concentration is 100° C., distillation, and the distillation conc...

Embodiment 2

[0032] A reduction preparation method of 4-trifluoromethylpiperidine, comprising the following steps:

[0033] (1) Preparation of 4-trifluoromethylpiperidine:

[0034] At room temperature, 4-trifluoromethylpyridine and Raney nickel are put into the reactor, the addition of Raney nickel catalyst is 8% of 4-trifluoromethylpyridine weight, feed hydrogen into the reactor and Maintain 3-12 atmospheric pressure, carry out hydrogenation under stirring, and carry out hydrogenation reduction reaction under the catalysis of Raney nickel to generate 4-trifluoromethylpiperidine, and the reaction is shown in formula 2.

[0035] (2) Purification of 4-trifluoromethylpiperidine:

[0036] The reaction mixture in step (1) was filtered to remove the catalyst, and the obtained filtrate was concentrated by distillation to remove ether. The temperature of the distillation concentration was 200 ° C. Distillation. The distillation concentration step used a rotary evaporator, and the concentrate was ...

Embodiment 3

[0039] A reduction preparation method of 4-trifluoromethylpiperidine, comprising the following steps:

[0040] (1) Preparation of 4-trifluoromethylpiperidine:

[0041] At room temperature, 4-trifluoromethylpyridine and Raney nickel are put into the reactor, the addition of Raney nickel catalyst is 15% of 4-trifluoromethylpyridine weight, feed hydrogen into the reactor and Maintain 3-12 atmospheric pressure, carry out hydrogenation under stirring, and carry out hydrogenation reduction reaction under the catalysis of Raney nickel to generate 4-trifluoromethylpiperidine, and the reaction is shown in formula 2.

[0042] (2) Purification of 4-trifluoromethylpiperidine:

[0043] The reaction mixture in the step (1) is filtered to remove the catalyst, and the obtained filtrate is concentrated by distillation to remove propylene glycol. The temperature of the distillation concentration is 150°C. Distillation. The distillation concentration step uses a rotary evaporator, and the conce...

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Abstract

The invention discloses a reduction preparation method of 4-(trifluoromethyl)piperidine, which is characterized by comprising the following steps of: forming the 4-(trifluoromethyl)piperidine through the hydrogenation reduction of 4-(trifluoromethyl)pyridine; and carrying out distillation and concentration on a reaction mixture, carrying out precipitation by using a solvent, and filtering, washing and drying to obtain the 4-(trifluoromethyl)piperidine. The reduction preparation method has the advantages of simple process, easiness in the obtaining of raw materials, and convenience in preparation.

Description

technical field [0001] The invention relates to a method for preparing 4-trifluoromethylpiperidine, in particular to a reduction preparation method of 4-trifluoromethylpiperidine, which belongs to the technical field of chemical industry. Background technique [0002] The registration number of 4-trifluoromethylpiperidine (4-(Trifluoromethyl)piperidine) is 657-36-3, 4-trifluoromethylpiperidine is an important chemical raw material. However, in the existing production, the raw materials are relatively expensive and the process is complicated, which limits the large-scale production of 4-trifluoromethylpiperidine. With the progress and development of the economy, the chemical industry has developed rapidly, providing many raw materials and intermediates for industry, agriculture and pharmaceutical industries, and widely used in the fields of medicine, dyes, oils, spices, and synthetic fibers. Contents of the invention [0003] In order to solve the above problems, the prese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/18
Inventor 柳叶谢西平
Owner SHANGHAI SINOFLUORO SCI
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