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Preparation method of azobenzene oxide

A technology of azobenzene oxide and compounds, which is applied in the field of preparation of azobenzene oxide, can solve the problems of large environmental pollution, high risk, and high cost, and achieve the effects of small environmental pollution, low cost, and novel methods

Active Publication Date: 2021-02-19
HUAIYIN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The current method for synthesizing azobenzene oxide requires strong base, strong acid, and reducing agent, which causes great environmental pollution, high cost, and great danger

Method used

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  • Preparation method of azobenzene oxide
  • Preparation method of azobenzene oxide
  • Preparation method of azobenzene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039]

[0040]Add the compound nitrobenzene (25mg, 0.2mmol) and LiClO to the dry 10mL two-necked chicken heart flask4(10.6mg, 0.1mmol), a rubber stopper at the mouth of a bottle passes through a platinum wire and a silver wire as a wire. The lower end of the wire is connected with two pieces of graphite felt (2cm×1cm×0.5cm). The sheets of graphite felt are separated by a Teflon film, and then the two sheets of graphite felt are tied tightly with a Teflon thread. The graphite felt connected by platinum wire is used as the anode for electrolysis reaction, and the graphite felt connected by silver wire is used as the cathode for electrolysis reaction. Fill the reaction flask with ammonia for 3 times and add 5mL dry CH3CN. The reaction was reacted at a constant voltage of 6V and room temperature, and the reaction was monitored by TLC and GC-MS. After about 4 hours of reaction, transfer the reaction stock solution, add ethyl acetate to wash, mix the stock solution with the washing solution...

Embodiment 2

[0043]

[0044]Add the compound o-fluoronitrobenzene (28mg, 0.2mmol) and LiClO to the dry 10mL two-necked chicken heart flask4(10.6mg, 0.1mmol), a rubber stopper at the mouth of a bottle passes through a platinum wire and a silver wire as a wire. The lower end of the wire is connected with two pieces of graphite felt (2cm×1cm×0.5cm). The sheets of graphite felt are separated by a Teflon film, and then the two sheets of graphite felt are tied tightly with a Teflon thread. The graphite felt connected by platinum wire is used as the anode for electrolysis reaction, and the graphite felt connected by silver wire is used as the cathode for electrolysis reaction. Fill the reaction flask with ammonia for 3 times and add 5mL dry CH3CN. The reaction was reacted at a constant voltage of 6V and room temperature, and the reaction was monitored by TLC and GC-MS. After about 4 hours of reaction, transfer the original reaction solution, add ethyl acetate to wash, mix the original solution with the wa...

Embodiment 3

[0047]

[0048]Add the compound o-trifluoromethylnitrobenzene (38mg, 0.2mmol) and LiClO to a dry 10mL two-necked chicken heart bottle in sequence4(10.6mg, 0.1mmol), a rubber stopper at the mouth of a bottle passes through a platinum wire and a silver wire as a wire. The lower end of the wire is connected with two pieces of graphite felt (2cm×1cm×0.5cm). The graphite felt is separated by a Teflon film, and the two graphite felts are tied tightly with a Teflon thread. The graphite felt connected by platinum wire is used as the anode for electrolysis reaction, and the graphite felt connected by silver wire is used as the cathode for electrolysis reaction. Fill the reaction flask with ammonia for 3 times and add 5mL dry CH3CN. The reaction was reacted at a constant voltage of 6V and room temperature, and the reaction was monitored by TLC and GC-MS. After about 4 hours of reaction, transfer the reaction stock solution, add ethyl acetate to wash, mix the stock solution with the washing solut...

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Abstract

The invention belongs to the technical field of organic synthesis, and discloses an azobenzene oxide preparation method, which comprises: S1, sequentially adding a nitrobenzene compound and an electrolyte to a dry two-neck heart-shaped bottle; S2, allowing a platinum wire to penetrate through a rubber plug of a vertical bottle opening to serve as a wire A and allowing another silver wire or platinum wire to penetrate through the rubber plug of the vertical bottle opening to serve as a wire B; and S3, connecting the end part of the wire A in S2 with graphite felt which is used as an electrolytic reaction anode, and connecting the end part of the wire B in the S2 with graphite felt which is used as an electrolytic reaction cathode, arranging a Teflon film between the two pieces of graphite felt, and tying the two pieces of graphite felt by using a Teflon wire. The method provided by the invention has the advantages of novelty, cheap and easily available raw materials, no need of strong base and reducing agent, small environmental pollution and low cost, and breaks through the problems of large raw material pollution, high cost and high risk of the traditional azobenzene oxide synthesis method.

Description

Technical field[0001]The invention belongs to the technical field of organic synthesis, and specifically relates to a method for preparing azobenzene oxide.Background technique[0002]Azobenzene oxide is also an important organic synthesis intermediate, and its production method is obtained by reducing nitrobenzene. Put nitrobenzene and sodium hydroxide solution into the reaction pot, raise the temperature to 60°C, slowly add glucose solution, and keep it at 65-75°C for 1h, that is, the reaction produces azobenzene oxide. Laboratory preparation example: In a 500ml flask with reflux device, add a solution of 30g sodium hydroxide and 100ml water, then add 20.5g pure nitrobenzene, heat in a water bath, and keep the temperature at 55-60℃. Under agitation, add 21g of anhydrous glucose in several times, and add it in about 1 hour. Heat in a boiling water bath for 2h. Then the hot reactant is steam distilled to remove unreacted nitrobenzene and reaction by-product aniline. When the distillat...

Claims

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Application Information

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IPC IPC(8): C25B3/29C25B3/09C25B3/07C07C291/08
CPCC07C291/08
Inventor 李进刘畅洪坤端木传嵩徐海青胡永珂
Owner HUAIYIN INSTITUTE OF TECHNOLOGY
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