Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method for bromopentafluorobenzene

A technology of pentafluorobromobenzene and pentafluorophenol, which is applied in the field of preparation of pentafluorobromobenzene, can solve the problems of low product yield, high temperature conditions, and harsh equipment requirements, and achieve short synthesis process flow, high purity and Yield, effect of reaction conditions and temperature

Inactive Publication Date: 2015-04-22
QINGDAO WUWEI THERMAL INSULATION MATERIAL
View PDF1 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to literature reports, using pentafluorobenzene as a raw material and liquid bromine to synthesize pentafluorobromobenzene through bromination reaction requires high temperature conditions and harsh equipment requirements, which is not conducive to industrial production; using pentafluorobenzene and N-bromobutane The conditions required for the synthesis of pentafluorobromobenzene by reaction of nitric acid imide (NBS) are relatively low, but the product yield is too low, which is also unfavorable for industrial production; Chinese patent CN102531832A, is prepared by two-step reaction of decarboxylation and bromination with pentafluorobenzoic acid Bromopentafluorobenzene has lower requirements on reaction conditions, but the process is longer and the operation is troublesome

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] A preparation method of pentafluorobromobenzene, including the following steps:

[0015] Put 55.2g of pentafluorophenol and 27.0g of phosphorus tribromide into a 250ml reaction flask and raise the temperature to 50-60°C, then add 10g of triphenylphosphine, and continue to heat up to 68-700°C for 1.5h; after the reaction, Cool down to 50~60℃ and keep for 30min; then put the reaction flask in an ice bath to cool to room temperature, filter, distill the filtrate, pass it into the condenser to condense to obtain pentafluorobromobenzene, the purity of the target product can reach 97.80%, The product yield can reach 69.0%.

Embodiment 2

[0017] A preparation method of pentafluorobromobenzene, including the following steps:

[0018] Put 92g of pentafluorophenol and 27.0g of phosphorus tribromide into a 250ml reaction flask to raise the temperature to 50-60°C, then add 15g of triphenylphosphine, and continue to raise the temperature to 68-70°C and react for 2h; after the reaction, cool to 50~60℃ and keep for 30min; then put the reaction flask into an ice bath to cool to room temperature, filter, distill the filtrate, pass it into the condenser to condense to obtain pentafluorobromobenzene, the purity of the target product can reach 98.40%, and the product yields The rate can reach 71.22%.

Embodiment

[0020] A preparation method of pentafluorobromobenzene, including the following steps:

[0021] Put 55.2g of pentafluorophenol and 27.0g of phosphorus tribromide into a 250ml reaction flask and raise the temperature to 50-60℃, then add 12g of triphenylphosphine, continue to heat up to 68~700℃ and react for 2h; after the reaction, cool down Heat to 50~60℃ and keep for 30min; then put the reaction flask in an ice bath to cool to room temperature, filter, distill the filtrate, pass it into the condenser to condense to obtain pentafluorobromobenzene, the purity of the target product can reach 98.92%, the product The yield can reach 71.56%.

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

A disclosed preparation method for bromopentafluorobenzene comprises: adding a certain amount of pentafluorophenol and phosphorous tribromide into a 250 mL reaction flask, heating to 50-60 DEG C, then adding a certain amount of a catalyst, continuing to heat to 60-90 DEG C for reacting for 1-2 h; and after the reaction is finished, cooling to 50-60 DEG C and keeping warm for 30-60 min, then putting the reaction flask into an ice bath to cool to room temperature, filtering, distillating the filtrate, and introducing into a condenser tube for condensing, so as to obtain bromopentafluorobenzene. The preparation method for bromopentafluorobenzene is easily available in raw materials, mild in reaction conditions, short in synthesis technological flow and simple in operation, the obtained target product has relatively high purity and yield, the product purity can reach 97%, and the product yield can reach 72%.

Description

Technical field [0001] The invention relates to a preparation method of pentafluorobromobenzene, which belongs to the field of fine chemicals. Background technique [0002] Pentafluorobromobenzene is a colorless to slightly yellow liquid. It is an important new type of fine chemical intermediate. It has a wide range of uses and development prospects. It can be used in the fields of medicine and pesticides, as well as in liquid crystal products, Catalyst intermediate for olefin polymerization. According to literature reports, the synthesis of pentafluorobromobenzene by bromination reaction with pentafluorobenzene as raw material and liquid bromine requires high temperature conditions and harsh equipment requirements, which is not conducive to industrial production; use pentafluorobenzene and N-bromobutanedi The synthesis of pentafluorobromobenzene by NBS reaction requires low conditions, but the product yield is too low, which is not conducive to industrial production; Chinese pa...

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
IPC IPC(8): C07C25/13C07C17/16
Inventor 李本明
Owner QINGDAO WUWEI THERMAL INSULATION MATERIAL
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com