Check patentability & draft patents in minutes with Patsnap Eureka AI!

Synthesis method of 3-bromopyridine

A synthesis method and technology of bromopyridine, applied in the field of synthesis of 3-bromopyridine, can solve the problems of low yield, expensive raw materials, and high requirements for reaction conditions, and achieve the effects of high yield, simple reaction steps, and easy-to-obtain raw materials

Inactive Publication Date: 2019-05-14
丹阳市中润检测技术有限公司
View PDF0 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is: to overcome the deficiencies of low yield, high requirements on reaction conditions and expensive raw materials in the prior art, and provide a kind of 3-bromine with high yield, mild reaction conditions, simple operation and suitable for industrialization The synthetic method of pyridine

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
  • Synthesis method of 3-bromopyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Drop 8.8g of bromine (50mmol) into 15ml (185mmol) and 95% sulfuric acid at 0℃, react at 130℃ for 8 hours, cool and pour into ice water after the reaction, adjust the pH to 8,60ml petroleum ether with 6N sodium hydroxide After three extractions, several layers were dried with anhydrous sodium sulfate after the layers were separated, the organic layer was concentrated after filtering the desiccant, and then distilled with a Vigro fractionation column. Analyze the composition of the remaining substances in the gas phase, the detection condition: N 2 90ml / min, H 2 120ml / min, column temperature 165°C, 4ul sample injection, yield 75%.

Embodiment 2

[0020] Drop 8.8g of bromine (50mmol) into 15ml (185mmol) and 80% sulfuric acid at 0℃, react at 130℃ for 8 hours, cool and pour into ice water after the reaction, adjust the pH to 8,60ml petroleum ether with 6N sodium hydroxide After three extractions, several layers were dried with anhydrous sodium sulfate after the layers were separated, the organic layer was concentrated after filtering the desiccant, and then distilled with a Vigro fractionation column. Analyze the composition of the remaining substances in the gas phase, the detection condition: N 2 90ml / min, H 2 120ml / min, column temperature 165°C, 4ul injection, yield 65%.

Embodiment 3

[0022] Drop 8.8g of bromine (50mmol) into 15ml (185mmol) and 90% sulfuric acid at 0°C, react at 130°C for 8 hours, cool and pour into ice water after the reaction, adjust the pH to 8,60ml petroleum ether with 6N sodium hydroxide It was extracted three times. After the layers were separated, several layers were dried with anhydrous sodium sulfate. After filtering the desiccant, the organic layer was concentrated, and then distilled by a Vigre column. Analyze the composition of the remaining substances in the gas phase, detection condition: N 2 90ml / min, H 2 120ml / min, column temperature 165°C, 4ul sample injection, yield 70%.

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 belongs to the field of organic synthesis, and particularly relates to a synthesis method of 3-bromopyridine. The invention includes following steps: (1), dropwise adding bromine into pyridine and sulfuric acid of 80-95% at 0 DEG C, and allowing reaction at 130-140 DEG C for 7-8h; (2), cooling after reaction is finished, pouring into ice water, and using 6N sodium hydroxide to adjustPH to 8; (3), using an organic solvent for extraction, layering, drying, filtering, concentrating, and distilling. The synthesis method has the advantages of being high in yield, mild in reaction condition, simple in reaction step, simple and easy-to-obtain in raw material and suitable for industrial production.

Description

Technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for synthesizing 3-bromopyridine. Background technique [0002] 3-Bromopyridine is commonly used as an intermediate in medicine, pesticide and organic synthesis. It can be used in the synthesis of 3-methylaminopiperidine, an intermediate of balofloxacin, a class of drugs. The synthetic methods of 3-bromopyridine are: (1) pyridine and aluminum trichloride are reacted with bromine; (2) 3-aminopyridine is brominated, then diazotized and then subjected to Sandmeyer reaction to obtain the product . Method (1) has great shortcomings, the yield is low, and the requirement for anhydrous during the reaction is very high and the salt formation is difficult to stir, and the bromination of pyridine hydrochloride salt is not very strong, and it is easy to generate bromine in other positions The chemical product brings a lot of trouble to the post-treatment, and the yield is not high. ...

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): C07D213/61
Inventor 魏倩
Owner 丹阳市中润检测技术有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com