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

Method for activating 3-bromopropyne

A technology of bromopropyne and propargyl alcohol, which is applied in the field of activating 3-bromopropyne, can solve problems such as unfavorable industrialization, activity reduction, and large-scale production constraints, and achieve the effect of good application prospects and good industrial production potential

Inactive Publication Date: 2018-12-07
盐城市胜达化工有限公司
View PDF4 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, bromine-containing medical chemical intermediates will decompose in a small amount. After decomposition, their activity will decrease, which will affect the use effect. From the perspective of industrial scale, the characteristics of the above-mentioned methods make large-scale production subject to certain restrictions, which is not conducive to industrialization.

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
  • Method for activating 3-bromopropyne
  • Method for activating 3-bromopropyne
  • Method for activating 3-bromopropyne

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0044] Add hydrogen bromide solvent to the reaction kettle, add CuBr and Cu catalyst, stir and heat in a sealed environment, and at the same time add propargyl alcohol for reaction, the temperature rises at 50 ° C ~ 70 ° C, and the reaction is carried out for 1-3 hours; in the above process, pass through the filter device Filter, and add silver bicarbonate powder; rectify to obtain finished product 3-bromopropyne; add silver bicarbonate powder again to obtain low-water finished product 3-bromopropyne with high activation and not easy to decompose, such as attached. figure 1 shown in the flowchart.

specific Embodiment 2

[0045] Add hydrogen bromide solvent to the reaction kettle, add CuBr and Cu catalyst, stir in a sealed environment, add a small amount of pyridine to the dry propargyl alcohol at the same time, and add phosphorus tribromide and a small amount of phosphorus tribromide at 0 °C under stirring. The pyridine solution was stirred for 20 minutes after dropping, and propargyl alcohol and silver bicarbonate powder were added to react, the temperature was raised, and the reaction was performed under reduced pressure for 2 hours to obtain the product 3-bromopropyne, wherein the vacuum distillation step included subjecting the oil layer to a high-efficiency rectifying tower Rectification, collecting 130-150 ℃ pressure (6.7kPa) fractional distillation, the product is 3-bromopropyne, and adding silver bicarbonate powder again to obtain low-water product 3-bromopropyne with high activation and not easy to decompose, such as attached figure 2 shown in the flowchart.

specific Embodiment 3

[0046] Add propargyl alcohol to pyridine under cooling, stir at -5 °C and slowly add phosphorus tribromide, the reaction temperature is maintained below 0 °C, after the addition, continue stirring for 15min, add silver bicarbonate powder, and distill under reduced pressure, wherein , the vacuum distillation step includes rectifying the oil layer with a high-efficiency rectifying tower, collecting 130-150 ° C, collecting all the distillate under the pressure (6.7kPa), and fractionating it again under normal pressure to obtain the finished product 3-bromopropyne , adding silver bicarbonate powder again to obtain 3-bromopropyne, a low-water product with high activation and not easy to decompose. image 3 shown in the flowchart.

[0047]In the present invention, because the chemical intermediate 3-bromopropyne with high purity is placed for a period of time, it will decompose in a small amount. After the decomposition, the activity equivalent to the pharmaceutical intermediate 3-b...

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 method for activating 3-bromopropyne. The method comprises the following steps: adding a hydrogen bromide solvent to a reaction kettle, adding CuBr and Cu catalysts, stirringand heating in a sealed environment, adding propargyl alcohol for producing a reaction, heating, and reacting; performing filtration by a filtering device during the step 1), and adding silver bicarbonate powder; obtaining finished 3-bromopropyne by rectification; and obtaining low-water finished product 3-bromopropyne which is highly activated and not easily decomposed by adding the silver bicarbonate powder again. According to the method, redundant bromide ions are removed by addition of the silver bicarbonate powder, so that the finished 3-bromopropyne becomes active and does not easily decompose.

Description

technical field [0001] The present invention relates to the field of chemical intermediates, in particular to a method for activating 3-bromopropyne. Background technique [0002] At present, the main uses of bromine resources in the world are roughly divided into: medicine and pharmaceutical intermediates 19%, flame retardants 32%, oilfield additives 11%, pesticides and pesticide intermediates 12%, dyes and dye intermediates 5%, water treatment agents 6% %, photographic chemicals and rubber additives 10%, other 5%. There are nearly 60 kinds of products that require bromine in the pharmaceutical and pharmaceutical intermediate industries. At present, the annual demand for bromine in the pharmaceutical industry is about 16,000 tons. With the improvement and progress of industrial technology, the market will gradually expand, and the pharmaceutical intermediates that consume bromine will have a greater development. 3-Bromopropyne, also known as 3-bromo-1-propyne; propargyl b...

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): C07C17/16C07C17/38C07C21/22
CPCC07C17/16C07C17/38C07C21/22
Inventor 周荣军陈士怀李标刘红霞
Owner 盐城市胜达化工有限公司
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