Supercharge Your Innovation With Domain-Expert AI Agents!

2,4-dinitroanisole synthesis method

A technology of dinitroanisole and synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as troublesome post-processing, long reaction time, large amount of reaction solvent, etc., and achieve the goal of reaction Mild conditions, no side reactions, high product purity

Inactive Publication Date: 2017-05-31
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
View PDF4 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although 2,4-dinitroanisole can be effectively synthesized by the above method, there are shortcomings such as long reaction time, large amount of reaction solvent, inability to recycle the mother liquor after the reaction, and a large amount of waste water generated by the reaction. Unavoidable generation of by-product 2,4-dinitrophenol, which affects the yield of the target product and brings trouble to post-processing
[0005] Publication No. CN103396318A discloses the method for preparing 2,4-dinitroanisole using methanol solution of sodium hydroxide and alkali metal oxides to replace sodium hydroxide aqueous solution, although it solves the problem of producing a large amount of waste water in the traditional process and mother liquor cannot be recycled, but in the reaction process, it is necessary to add other alkali metal salts, such as magnesium oxide and calcium oxide, which increases the cost of raw materials, and this method does not solve the problem of by-product 2,4-dinitrophenol generated questions

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
  • 2,4-dinitroanisole synthesis method
  • 2,4-dinitroanisole synthesis method
  • 2,4-dinitroanisole synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023]

[0024] Add 2,4-dinitrochlorobenzene (5.0g, 25.0mmol) and methanol (5mL) into a 100mL two-necked reaction flask, raise the temperature to an internal temperature of 40°C (feeding temperature), stir until the solids are completely dissolved, and add 4.7g 30% by mass concentration of sodium methoxide in methanol solution (containing 1.4 g of sodium methoxide, 1.02 equiv., 25.5 mmol), dripped in 20 minutes. After dropping, the temperature was raised to an internal temperature of 60°C (reaction temperature), and the reaction was carried out for 7 hours until the pH value of the reaction solution was 8-9, and the reaction was stopped. Filtration, the filter cake was washed with water 4 times (4x5mL), the solid was collected and vacuum-dried to obtain light yellow solid 2,4-dinitroanisole (4.69g, yield 95.8%), detected by HPLC, the product purity was greater than 99% %.

Embodiment 2

[0026] The reaction steps and operations are the same as in Example 1, except that the molar ratio of 2,4-dinitrochlorobenzene to sodium methoxide in the reaction is 1:1. The reaction was stopped, and 2,4-dinitroanisole (4.63 g, yield 94.5%) was obtained after post-processing. The purity of the product was greater than 99% as detected by HPLC.

Embodiment 3

[0028] The reaction steps and operations are the same as in Example 1, except that the molar ratio of 2,4-dinitrochlorobenzene to sodium methoxide in the reaction is 1:2. The reaction was stopped, and 2,4-dinitroanisole (4.20 g, yield 85.7%) was obtained after post-processing. The purity of the product was greater than 99% as detected by HPLC.

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 present invention discloses a 2,4-dinitroanisole synthesis method, wherein 2,4-dinitrochlorobenzene is adopted as a raw material, methanol is adopted as a solvent, and 2,4-dinitrochlorobenzene reacts with sodium methoxide under a mild condition to synthesize 2,4-dinitroanisole. Compared to the reported 2,4-dinitroanisole synthesis method, the2,4-dinitroanisole synthesis method of the present invention has advantages of low raw material cost, mild reaction condition, simple operation, high reaction efficiency, no side reaction occurrence, high product purity, and the like.

Description

technical field [0001] The invention relates to a synthesis method of 2,4-dinitroanisole. The method uses 2,4-dinitrochlorobenzene as a raw material, methanol as a solvent, and reacts with sodium methoxide under mild conditions to synthesize 2,4-dinitroanisole. Compared with the reported synthesis method of 2,4-dinitroanisole, the present invention has the advantages of low raw material cost, mild reaction conditions, simple operation, high reaction efficiency, no side reaction and high product purity. Background technique [0002] 2,4-Dinitroanisole (CAS: 119-27-7) is an important fine chemical or organic intermediate, which is not only an effective insecticide, but also a raw material for synthetic dyes, medicines and pesticides , so it is of great significance to develop a simple and effective method for the synthesis of 2,4-dinitroanisole. [0003] The Chinese patent application whose publication number is CN1146450A discloses a method for preparing 2,4-dinitroanisole ...

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): C07C205/37C07C201/12
CPCC07C201/12C07C205/37
Inventor 余正坤吴凯凯
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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