P-chlorobenzotrifluoride clean nitration reaction catalyzed by heteropoly acid ionic liquid

A technology of p-chlorotrifluorotoluene and ionic liquid, which can be used in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry and other directions, and can solve the problems of difficult separation and purification, environmental hazards and high cost , to achieve the effect of wide source of raw materials, high catalytic activity and convenient preparation

Inactive Publication Date: 2012-04-18
YANCHENG TEACHERS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high cost of imidazole-type ionic liquids, it is not conducive to large-scale application
In addition, a series of studies have shown (Garcia M T, Gathergood N, Scammells P J. Biodegradable ionic liquids Part II. Effect of the anion and toxicology. Green Chem. 2005, 7: 9-14), based on imidazole, pyridinium cation type The biodegradability of ionic liquid is very poor, and it is not easy to degrade through the

Method used

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  • P-chlorobenzotrifluoride clean nitration reaction catalyzed by heteropoly acid ionic liquid
  • P-chlorobenzotrifluoride clean nitration reaction catalyzed by heteropoly acid ionic liquid
  • P-chlorobenzotrifluoride clean nitration reaction catalyzed by heteropoly acid ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 25mL round bottom flask, add 10mmol (1.81g) p-chlorobenzotrifluoride, 30mmol (2.8g) 65% nitric acid, 1.0mmol catalyst (the anion is H 2 PMo 12 o 40 - ), mixed and stirred for 10 hours at 80° C., cooled, and allowed to stand for phase separation. The crude product in the upper layer was washed with water, neutralized, and vacuum-dried to obtain the pure product 4-chloro-3-nitrobenzotrifluoride, with a yield of 80%.

Embodiment 2

[0024] In a 25mL round bottom flask, add 10mmol (1.81g) p-chlorobenzotrifluoride, 20mmol (1.26g) 100% nitric acid, 0.5mmol catalyst (the anion is H 2 PMo 12 o 40 - ), mixed and stirred for 1 hour at 20° C., cooled, and allowed to stand for phase separation. The crude product in the upper layer was washed with water, neutralized, and vacuum-dried to obtain the pure product 4-chloro-3-nitrobenzotrifluoride, with a yield of 83%.

Embodiment 3

[0026] In a 25mL round bottom flask, add 10mmol (1.81g) p-chlorobenzotrifluoride, 10mmol (0.63g) 100% nitric acid, 0.5mmol catalyst (the anion is H 2 PMo 12 o 40 - ), mixed and stirred for 5 hours at 50° C., cooled, left to stand for phase separation, and the crude product in the upper layer was washed with water, neutralized and dried in vacuo to obtain the pure product 4-chloro-3-nitrobenzotrifluoride, with a yield of 95%.

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Abstract

The invention discloses a novel method for carrying out p-chlorobenzotrifluoride clean nitration reaction catalyzed by a heteropoly acid ionic liquid. The used catalyst is an ionic liquid having a heteropoly acid anionic structure, and p-chlorobenzotrifluoride and nitric acid used as raw materials are subjected to nitration reaction under the action of the catalyst, thus obtaining 4-chloro-3-nitrobenzotrifluoride. Compared with the prior art, the invention has the following advantages: (1) the used ionic liquid having a heteropoly acid anionic structure has a wide source of raw materials and is convenient to prepare; and the catalyst is stable in water, can not be inactivated and can be used circularly; (2) compared with corresponding inorganic acid, the heteropoly acid forming the anionic structure has higher strength, higher catalytic activity, less consumption and better environment friendliness; and (3) by using the ionic liquid instead of concentrated sulfuric acid, the nitration process is environment-friendly and has industrial application prospects.

Description

a technical field [0001] The invention relates to a new method for catalyzing the clean nitration reaction of p-chlorobenzotrifluoride by a heteropolyacid ionic liquid, and belongs to the technical field of chemical material preparation. The method is applicable to the occasion of synthesizing 4-chloro-3-nitrobenzotrifluoride with p-chlorobenzotrifluoride and nitric acid as raw materials by heating and stirring under normal pressure. Two background technology [0002] Nitrification is an important unit reaction of organic synthesis, and substituted aromatic nitrates are a very important class of chemical products. The methods and processes of nitration of aromatic compounds have been studied in both academia and industry. Energy saving and emission reduction is an important issue faced by human beings, and the clean nitrification of aromatic compounds has become one of the hotspots of people's research. [0003] The nitrated product of p-chlorobenzotrifluoride, 4-chloro-3-n...

Claims

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Application Information

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IPC IPC(8): C07C205/12C07C201/08B01J31/18
Inventor 方东郑龙洲张根成谢毅
Owner YANCHENG TEACHERS UNIV
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