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A kind of preparation method of azobenzene oxide

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

Active Publication Date: 2022-01-28
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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  • A kind of preparation method of azobenzene oxide
  • A kind of preparation method of azobenzene oxide
  • A kind of preparation method of azobenzene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039]

[0040] Add compound nitrobenzene (25mg, 0.2mmol), LiClO 4 (10.6mg, 0.1mmol), a rubber stopper at the mouth of a bottle passes through a platinum wire and a silver wire as wires, and the lower ends of the wires are respectively connected with two pieces of graphite felt (2cm×1cm×0.5cm). The middle of the graphite felt is separated by a Teflon film, and then the two graphite felts are fastened with a Teflon thread. The graphite felt connected with platinum wire is used as the anode of the electrolysis reaction, and the graphite felt connected with the silver wire is used as the cathode of the electrolysis reaction. The reaction flask was filled with ammonia gas 3 times, and then 5 mL of dry CH was added. 3 CN. The reaction was performed at a constant voltage of 6V at 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 t...

Embodiment 2

[0043]

[0044] Add compound o-fluoronitrobenzene (28mg, 0.2mmol), LiClO 4 (10.6mg, 0.1mmol), a rubber stopper at the mouth of a bottle passes through a platinum wire and a silver wire as wires, and the lower ends of the wires are respectively connected with two pieces of graphite felt (2cm×1cm×0.5cm). The middle of the graphite felt is separated by a Teflon film, and then the two graphite felts are fastened with a Teflon thread. The graphite felt connected with platinum wire is used as the anode of the electrolysis reaction, and the graphite felt connected with the silver wire is used as the cathode of the electrolysis reaction. The reaction flask was filled with ammonia gas 3 times, and then 5 mL of dry CH was added. 3 CN. The reaction was performed at a constant voltage of 6V at 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 solutio...

Embodiment 3

[0047]

[0048] Add compound o-trifluoromethylnitrobenzene (38mg, 0.2mmol), LiClO 4 (10.6mg, 0.1mmol), a rubber stopper at the mouth of a bottle passes through a platinum wire and a silver wire as wires, and the lower ends of the wires are respectively connected with two pieces of graphite felt (2cm×1cm×0.5cm). The middle of the graphite felt is separated by a Teflon film, and then the two graphite felts are fastened with a Teflon thread. The graphite felt connected with platinum wire is used as the anode of the electrolysis reaction, and the graphite felt connected with the silver wire is used as the cathode of the electrolysis reaction. The reaction flask was filled with ammonia gas 3 times, and then 5 mL of dry CH was added. 3 CN. The reaction was performed at a constant voltage of 6V at 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 origina...

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Abstract

The invention belongs to the technical field of organic synthesis, and discloses a preparation method of azobenzene oxide, comprising the following steps: S1. Adding nitrobenzene compounds and electrolytes to a dry two-necked chicken heart bottle in sequence; S2. Rubber on the vertical bottle mouth Plug through a platinum wire as wire A and another silver wire or platinum wire as wire B; S3. Connect the end of wire A of S2 to a piece of graphite felt, which is used as the electrolytic reaction anode; wire B of S2 A piece of graphite felt is connected to the end, and this graphite felt is used as the cathode of the electrolysis reaction. There is a Teflon film between the two pieces of graphite felt, and then the two pieces of graphite felt are fastened with Teflon wire. The method provided by the present invention has the advantages of novel method, cheap and easy-to-obtain raw materials, no need to use strong alkali and reducing agent, less environmental pollution and low cost, and a breakthrough in the traditional method for synthesizing azobenzene oxide with large raw material pollution, high cost and danger high question.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of azobenzene oxide. Background technique [0002] Azobenzene oxide is also an important intermediate in organic synthesis, 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, keep warm at 65-75°C for 1 hour, and react to form azobenzene oxide. Laboratory preparation example: In a 500ml flask with a reflux device, add a solution made 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°C. Under stirring, add anhydrous glucose with a total amount of 21 g several times, and the addition is completed in about 1 hour. Heated in a boiling water bath for 2h. The heated reactants are then subjected to steam distillation to re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C291/08C25B3/29C25B3/09C25B3/07
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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