Novel synthesis process of high-purity pesticide intermediate

A new process and synthesis method technology, applied in organic chemistry and other directions, can solve the problems of difficult production, high pollution, low yield, etc. Effect

Inactive Publication Date: 2012-07-25
ANHUI FENGLE AGROCHEM
View PDF3 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The method provided by the present invention then uses the mixed system instead of the traditional methanol single system, adopts a crystallization method to obtain high-purity 2-amino-4-chloro-6-methoxypyrimidine products, and imp...

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

example 1

[0015] Example 1: Add 16.8g of dichloropyrimidine (0.1mol), 100ml of methanol and 80ml of petroleum ether into a 250ml four-neck flask, stir and heat up to 40-50°C, quickly dropwise add 18.2g of sodium methoxide solution (0.101mol), and react After 2 hours, cool down and add 2g of diatomaceous earth, continue to reflux for 1 hour, heat filter, wash the filter cake, combine and cool the filtrate to 0-10°C to crystallize, filter with suction, apply the filtrate mechanically, and wash the filter cake with water to obtain 14.1g of white needle-shaped crystals. The content is 99.7%, and the molar yield is 88.1%.

example 2

[0016] Example 2: Add 16.8g of dichloropyrimidine (0.1mol) to a 250ml four-neck flask, recover about 170ml of mother liquor, 5ml of methanol and 5ml of petroleum ether in "Example 1", stir and heat up to 40-50°C, quickly dropwise add 18.2g sodium methoxide solution (0.101mol), react for 2 hours, cool down and add 2g of diatomaceous earth, continue to reflux for 1 hour, heat filter, wash the filter cake, combine the filtrates and cool down to 0-10°C to crystallize, suction filter, apply the filtrate mechanically, filter After the cake was washed with water, 14.62 g of white needle-like crystals were obtained, with a content of 99.3%, and a molar yield of 91.01%.

[0017] Example 3: Add 16.8g of dichloropyrimidine (0.1mol) to a 250ml four-neck flask, recover about 170ml of mother liquor, 5ml of methanol and 5ml of petroleum ether in "Example 2", stir and heat up to 40-50°C, quickly dropwise add 18.2g of sodium methoxide solution (0.101mol), react for 2 hours, cool down and add 2...

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 novel synthesis process of a chlorimuron-ethyl intermediate, i.e., high-purity 2-amino-4-chlorin-6-methoxypyrimidine (chloropyrimidine for short). The process comprises the following steps of: adding 2-amino-4,6-dichloropyrimidine (dichloropyrimidine for short) into a mixed solvent; raising the temperature and dropwise adding sodium methoxide; after reacting, adding a decolorizing agent; filtering, cooling, crystalizing and washing to obtain a high-purity target; and after a mixed mother solution is used for sufficient batches, performing distillation treatment. Due to the adoption of the process, the yield and total yield level of a high-purity product are increased, and the production difficulty is lowered greatly; and a high-end chlorimuron-ethyl product synthesized by using the high-purity chloropyrimidine intermediate produced with the process has strong competitive strength in domestic and international markets.

Description

Technical field: [0001] The invention relates to a production process of a chlorimuron-methyl intermediate, in particular to a new process for the preparation of high-purity 2-amino-4-chloro-6-methoxypyrimidine. Background technique: [0002] Chlorimuron-methyl is a selective pre-emergence and post-emergence herbicide, which can be absorbed by plant roots, stems, and leaves, conducts up and down in the plant body, and exerts herbicidal effect on vigorously growing meristem cells. It is mainly used in soybean fields Control broadleaf weeds. [0003] At present, the process commonly used in China is to react 2-amino-4,6-dichloropyrimidine with sodium methoxide in a methanol system. After the reaction is completed, the methanol is distilled, and then crystallized with water to obtain khaki powder particles with a content of 95-97%. That is a crude chloropyrimidine. Then use toluene or ethylene dichloride as a solvent, decolorize activated carbon, and then cool down to crystal...

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): C07D239/47
Inventor 苏朝辉周康伦沈良红王治民陈克付
Owner ANHUI FENGLE AGROCHEM
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