Preparation method of 1, 1 '-ethylene-2, 2'-dipyridyl dichloride

A bipyridine dichloride and bipyridine technology, applied in the field of chemical synthesis, can solve the problems of long reaction route, high cost, complicated process and the like, and achieve the effects of short reaction route, overcoming long reaction route and simple process

Active Publication Date: 2021-03-16
NANJING REDSUN BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] The present invention aims at the deficiencies such as long reaction route, complex process and high cost in the existing technology for preparing diquat dichloride, and provides a 1,1' -The preparation method of ethylene-2,2'-dipyridine dichloride

Method used

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  • Preparation method of 1, 1 '-ethylene-2, 2'-dipyridyl dichloride
  • Preparation method of 1, 1 '-ethylene-2, 2'-dipyridyl dichloride
  • Preparation method of 1, 1 '-ethylene-2, 2'-dipyridyl dichloride

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Add 360g of 2,2'-bipyridine and 3600g of dichloroethane into a dry 5L reactor, start stirring, replace the reactor with nitrogen, slowly raise the temperature to 130°C, raise the reaction pressure to 0.3MPa, keep at 130°C for 48h, and stop the reaction . Sampling analysis showed that the conversion rate of 2,2'-bipyridine was 4.1%, and the selectivity of the product 1,1'-ethylene-2,2'-bipyridine dichloride was 93.0%.

Embodiment 2

[0044] Add 360g of 2,2'-bipyridine and 3600g of dichloroethane into a dry 5L reactor, start stirring, replace the reactor with nitrogen, slowly raise the temperature to 250°C, raise the reaction pressure to 2.8MPa, keep at 250°C for 20h, and stop the reaction . Sampling analysis showed that the conversion rate of 2,2'-bipyridine was 58.2%, and the selectivity of the product 1,1'-ethylene-2,2'-bipyridine dichloride was 89.3%.

Embodiment 3

[0046] Add 360g of 2,2'-bipyridine and 3600g of dichloroethane into a dry 5L reactor, start stirring, replace the reactor with nitrogen, slowly raise the temperature to 290°C, raise the reaction pressure to 3.3MPa, keep at 290°C for 1 hour, and stop the reaction . Sampling analysis showed that the conversion rate of 2,2'-bipyridine was 30.2%, and the selectivity of the product 1,1'-ethylene-2,2'-bipyridine dichloride was 76.3%.

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Abstract

The invention discloses a preparation method of 1, 1 '-ethylene 2, 2'-dipyridyl dichloride, which comprises the following steps: by using 2, 2 '-dipyridyl and dichloroethane as raw materials and a solvent A or a solvent B as a solvent, carrying out cyclization reaction at 120-300 DEG C to obtain 1, 1'-ethylene 2, 2 '-dipyridyl dichloride, wherein the solvent A is selected from dichloroethane; thesolvent B meets the following conditions: (1) the solvent B does not chemically react with reaction raw materials or reaction products; 2, reaction raw materials of dichloroethane and 2, 2 '-dipyridylcan be dissolved; compared with the prior art, the method has the advantages of simple process, short reaction route and low cost, and is suitable for industrial production. The catalyst is added into the reaction system, so that the reaction rate can be remarkably increased, and the raw material conversion rate and the target product selectivity are improved.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a preparation method of 1,1'-ethylene-2,2'-bipyridine dichloride (diquat dichloride), in particular to a 2,2'- The invention discloses a method for preparing 1,1'-ethylene-2,2'-bipyridine dichloride with bipyridine and dichloroethane as raw materials. Background technique [0002] 1,1'-Ethylene-2,2'-bipyridine dibromide, diquat dibromide, was first developed by the predecessor of Syngenta, Imperial Chemical Industries (ICI). It is an excellent contact desiccant and herbicide with systemic properties. It is also one of the most widely used herbicide products in the world. The global sales and usage are second only to glyphosate, paraquat and glufosinate. . [0003] Patents US2823987 and GB815348 point out that diquat anion (C1 - ,Br - , I - , SO 4 2- ) change does not destroy its herbicidal activity. Literature (The dipyridylium herbicides, paraquat and diquat, P99; J.Sci.F...

Claims

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Application Information

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IPC IPC(8): C07D471/14
CPCC07D471/14
Inventor 薛谊陈洪龙王红伟杜翔王福军蒋剑华岳瑞宽罗超然王文魁
Owner NANJING REDSUN BIOCHEM CO LTD
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