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Method for preparing p-aminophenylacetonitrile by reducing p-nitrobenzeneacetonitrile by utilizing ammonium thiosulfate

A technology of p-nitrophenylacetonitrile and p-aminophenylacetonitrile, which is applied in the field of preparation of p-aminophenylacetonitrile, can solve the problems of low cost, unfavorable operators and environment, and low reduction efficiency of the alkali sulfide reduction method, and achieve low production cost, Environmental friendliness and less pollution effect

Inactive Publication Date: 2014-08-13
苏州久王环保科技股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005]Among the various methods of nitro reduction, the iron powder reduction method has always been the most widely used traditional method, but the iron filings reduction method will produce a large amount of iron sludge , seriously pollute the environment; the zinc powder reduction method is also widely applicable, but the zinc salt waste residue produced in production still needs to be treated separately; the cost of the alkali sulfide reduction method is low, but its reduction efficiency is not high, and harmful gases will be released during the reaction , which is not good for the operator and the environment
Therefore, the above methods are all limited because they will cause serious environmental pollution, prompting people to explore new and more environmentally and economically beneficial production methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a four-neck flask, add 1g of compound (1): p-nitrophenylacetonitrile, then add 20ml of ethanol and 10ml of water, start heating and stirring at a temperature of 80°C; after it is completely dissolved, add 6g of ( NH 4 ) 2 S 2 o 3 , to make it completely dissolved, and reflux reaction at 80°C for 4 hours; after 4 hours, the reaction stopped, and naturally cooled to room temperature, white crystals precipitated, and the precipitated crystals were filtered by suction, and compound (2) was obtained after complete drying: p-aminophenylacetonitrile , weighed 0.67g, and the yield was about 82.2%.

Embodiment 2

[0025] In a four-necked bottle, add 1g of compound (1): p-nitrophenylacetonitrile, then add 80ml of ethanol and 40ml of water, start heating and stirring, the heating temperature is 80°C; after it is completely dissolved, add 6g of ( NH 4 ) 2 S 2 o 3 , to make it completely dissolved, and reflux reaction at 80°C for 4 hours; after 4 hours, the reaction stopped, and naturally cooled to room temperature, white crystals precipitated, and the precipitated crystals were filtered by suction, and compound (2) was obtained after complete drying: p-aminophenylacetonitrile . The weighed was 0.62 g and the yield was about 76.1%.

Embodiment 3

[0027] In a four-neck flask, add 1g of compound (1): p-nitrophenylacetonitrile, then add 200ml of ethanol and 80ml of water, start heating and stirring at 80°C; after all of it is dissolved, add 6g of ( NH 4 ) 2 S 2 o 3 , to make it completely dissolved, and reflux reaction at 80°C for 4 hours; after 4 hours, the reaction stopped, and naturally cooled to room temperature, white crystals precipitated, and the precipitated crystals were filtered by suction, and compound (2) was obtained after complete drying: p-aminophenylacetonitrile , weighed 0.63g, and the yield was about 77.3%.

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PUM

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Abstract

The invention discloses a method for preparing p-aminophenylacetonitrile by reducing p-nitrobenzeneacetonitrile by utilizing ammonium thiosulfate. The method comprises the following steps: putting p-nitrobenzeneacetonitrile into a mixed solution of an organic solvent and water and stirring p-nitrobenzeneacetonitrile until p-nitrobenzeneacetonitrile is totally dissolved; adding ammonium thiosulfate and carrying out reflux reaction after heating and stirring; naturally cooling the reactant to the room temperature after reaction is stopped, precipitating a solid and leaching and drying the precipitated solid, thus obtaining the final product, namely p-aminophenylacetonitrile. The method is lower in production cost, is convenient and safe to operate, is environment-friendly, is simple in equipment and is suitable for continuous production.

Description

technical field [0001] The invention relates to a method for preparing p-aminophenylacetonitrile by reducing p-nitrophenylacetonitrile with ammonium thiosulfate. Background technique [0002] In the process of desulfurization and decyanation of coking gas purification, waste liquid will be produced. The inorganic salt ammonium thiosulfate recovered through the harmless treatment of waste liquid has a wide range of uses. It can be used as a fixer for photography, for plating Silver electroplating solution, metal cleaning agent, reducing agent, complexing agent, aluminum-magnesium alloy casting protection agent and chemical reagent. [0003] p-Nitrophenylacetonitrile is an important pharmaceutical intermediate for the lipid-lowering drug bezafibrate, the β-adrenergic receptor blocker atenolol, and the antidepressant Venlafxin (Venlafxin), and is also used in the preparation of Agrochemicals and liquid crystals can also be used to prepare azo dyes. In addition, p-nitrophenyla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/42C07C253/30
Inventor 张超智
Owner 苏州久王环保科技股份有限公司
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