Herbicide intermediate 3-chloro-2-methyl aniline production process

A technology of methylaniline and production process, which is applied in the field of preparation of pesticide intermediates, can solve the problems of three wastes, harsh conditions, and low yield, and achieve the effects of simple feeding and post-treatment, safe and mild reaction conditions, and high yield

Inactive Publication Date: 2008-10-22
ZHEJIANG UNIV
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned synthetic processes or catalysts are complicated to prepare, and the conditions are harsh, or many experimental processes involve high pressure conditions, low yield, low purity, complicated post-treatment, and many wastes, etc.

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
  • Herbicide intermediate 3-chloro-2-methyl aniline production process
  • Herbicide intermediate 3-chloro-2-methyl aniline production process
  • Herbicide intermediate 3-chloro-2-methyl aniline production process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In the 1000 milliliter three-necked flask, add 500 milliliters of N,N-dimethylacetamide solvent successively, 51 grams (0.3 moles) 2-chloro-6-nitrotoluene, 29 grams (0.9 moles, 3 equivalents) sulfur, 76 grams of sodium bicarbonate (0.9 moles, 3 equivalents), stirred and reacted at 130°C for 20 hours, terminated the reaction, then filtered, and the filtrate was fractionated under reduced pressure to obtain light yellow liquid 3-chloro-2-methylaniline, boiling point: 115~117 °C (10mmHg), yield 80%, purity 99% (GC).

Embodiment 2

[0021] In the 1000 milliliter three-necked flask, add 500 milliliters of N,N-dimethylacetamide solvent successively, 51 grams (0.3 moles) 2-chloro-6-nitrotoluene, 48 grams (1.5 moles, 5 equivalents) sulfur, 126 grams of sodium bicarbonate (1.5 moles, 5 equivalents), stirred and reacted at 110°C for 10 hours, ended the reaction, then filtered, and the filtrate was fractionated under reduced pressure to obtain light yellow liquid 3-chloro-2-methylaniline, boiling point: 115~117 °C (10mmHg), yield 77%, purity 99% (GC).

Embodiment 3

[0023] In the 1000 milliliter three-necked flask, add 500 milliliters of N,N-dimethylacetamide solvent successively, 51 grams (0.3 moles) 2-chloro-6-nitrotoluene, 29 grams (0.9 moles, 3 equivalents) sulfur, 76 grams of sodium bicarbonate (0.9 moles, 3 equivalents), stirred and reacted at 140°C for 24 hours, terminated the reaction, then filtered, and the filtrate was fractionated under reduced pressure to obtain light yellow liquid 3-chloro-2-methylaniline, boiling point: 115~117 °C (10mmHg), yield 85%, purity 99% (GC).

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 manufacturing technology of herbicide intermediate 3-chloride-2-methylaniline, which comprises the following steps: adopting N, N-dimethyl formamide as reacting solvent; stirring 2-chloride-6-nitrotoluene, sulfur and sodium hydrogen carbonate at 110-140 Deg C for 10-24h; filtering; decompressing filtrate; fractionating to obtain 3-chloride-2-nitrotoluene; setting the molar rate of 3-chloride-2-nitrotoluene and sulphur at 1: 3-5; making the quantity of sodium hydrogen carbonate as 3-5 times as 3-chloride-2-nitrotoluene.

Description

technical field [0001] The invention relates to a preparation method of a pesticide intermediate, in particular to a production process of a herbicide intermediate 3-chloro-2-methylaniline. Background technique [0002] 3-Chloro-2-methylaniline is an important pesticide intermediate, which can be used to synthesize hormone-type quinolinecarboxylic acid herbicides. The herbicide is widely used for pre-emergence and post-emergence weeding in direct seeded rice fields or transplanted rice fields, and can effectively control barnyard grass, saponin and other weeds. 3-Chloro-2-methylaniline is used as a raw material for the synthesis of quinclorac, and its purity directly affects the yield, content and efficacy of the synthetic quinclorac. Therefore, how to efficiently synthesize 3-chloro-2-methylaniline has attracted great attention. The synthesis of 3-chloro-2-methylaniline has been reported in some literatures. The literature "Pesticides" 2005 fourth phase, page 167 uses 2-...

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
Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/52C07C209/36
Inventor 林旭锋王晶
Owner ZHEJIANG UNIV
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