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Method for obtaining ketone through methylene oxidation

A methylene and oxidation system technology, applied in the chemical industry, can solve the problems of high production cost and high risk factor, and achieve the effect of environmental friendliness and low energy consumption

Inactive Publication Date: 2016-08-17
NANYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for oxidizing ketones through methylene, aiming to solve the problems of high risk factor and high production cost in the existing method of obtaining ketone compounds through oxidation

Method used

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  • Method for obtaining ketone through methylene oxidation
  • Method for obtaining ketone through methylene oxidation
  • Method for obtaining ketone through methylene oxidation

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0061] Diphenylmethane 1a (1.68g), sodium tert-butoxide (960mg), 18-crown-6 (2.64g) were added to a 100ml reaction flask, and then 20mL of N,N-dimethylformamide was added , followed by the introduction of one atmosphere of oxygen. Finally, the mixture was allowed to react at 20°C for 2 hours. After the reaction was completed, N,N-dimethylformamide was distilled off under reduced pressure, and then distilled under reduced pressure to obtain the product benzophenone 4a (1.8 g).

[0062]

example 2

[0064] Diphenylmethane 1a (168g), sodium tert-butoxide (120g), and 18-crown-6 (280g) were added to a 5-liter reaction flask respectively, and then 5L of N,N-dimethylformamide was added, followed by Oxygen at one atmosphere is introduced. Finally, the mixture was allowed to react at 20°C for 4 hours. After the reaction was completed, N,N-dimethylformamide was distilled off under reduced pressure, and then distilled under reduced pressure to obtain the product benzophenone 4a (150 g).

example 3

[0066]Benzophenone 2a (196g), potassium tert-butoxide (130g), and 18-crown-6 (300g) were added to a 5-liter reaction flask respectively, and then 100L of N,N-dimethylformamide was added, Oxygen at an atmospheric pressure is then introduced. Finally, the mixture was allowed to react at 50°C for 5 hours. After the reaction was completed, N,N-dimethylformamide was distilled off under reduced pressure, and then diphenyl ketone 5a (190 g) was obtained through distillation under reduced pressure.

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[0069]

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Abstract

The invention discloses a method for oxidizing ketones via methylene. The specific reaction system is as follows: the amount of methylene compound used is 0.01-500 mol; the pressure of oxygen used is 1-50 atmospheres; the amount of alkali used is methylene 1-2 times the equivalent of the moles of the compound; the amount of 18-crown-6 crown ether is 1-2 times the equivalent of the moles of the methylene compound; N,N-dimethylformamide or N,N-dimethyl The addition of acetamide makes the concentration of the methylene compound be 0.1-5mol / L; the reaction temperature is 0-100 degrees Celsius. The method for oxidation of methylene to ketone of the present invention can recycle used crown ether and water, has low energy consumption, no by-products of acid and metal salt are produced, and is environmentally friendly.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a method for oxidation of methylene to ketone. Background technique [0002] As a very important chemical raw material in organic chemical industry, ketone compounds have shown their special uses in many fields. Due to the importance of ketones, there are many different synthetic methods reported on the synthesis of ketones. The classic method for synthesizing ketones is the Friedel-Crafts acylation reaction of aromatic hydrocarbons and acyl halides or acid anhydrides, but this method will produce a large amount of solid by-products after the reaction, causing environmental pollution. [0003] In recent years, with the development of science and technology, people began to try to use active methylene compounds as raw materials to obtain ketone compounds by oxidation. At present, the commonly used method is peroxide oxidation, or a combination of transition metal compounds and w...

Claims

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Application Information

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IPC IPC(8): C07C45/36C07C49/786C07C49/784C07C49/78
CPCC07C45/36
Inventor 徐坤王会巧
Owner NANYANG NORMAL UNIV