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
View PDF0 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Reduction preparation method of 4-(trifluoromethyl)piperidine
  • Reduction preparation method of 4-(trifluoromethyl)piperidine
  • Reduction preparation method of 4-(trifluoromethyl)piperidine

Examples

Experimental program
Comparison scheme
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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/18
Inventor 柳叶谢西平
Owner SHANGHAI SINOFLUORO SCI
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap