Method for producing oxime

A solvent and organic peroxide technology, which is applied in the preparation of oximes, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of unstable industrial production and unsatisfactory methods, and achieve stable selectivity and yield. rate effect

Inactive Publication Date: 2010-01-20
SUMITOMO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, hydrogen peroxide is not necessarily cost-effective
Therefore, a method using organic peroxides as recyclable peroxides has been studied, but this method is not always satisfactory because the selectivity or yield of oxime is not stable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 1 L autoclave (reactor), 158.7 g of acetonitrile solution containing 2.6% by weight of ammonia, 7.6 g of cumene solution containing 80% by weight of cumene hydroperoxide and 5.0 g of Ti-MWW (via prepared in the same manner as described in Chemistry Letters, 2000, pp. 774-775), and replaced the gas phase part of the reactor with nitrogen. After the reactor was sealed, the temperature in the reactor was raised to 110° C. with stirring. The pressure in the reactor was 0.5 MPa. Next, 10 g of an acetonitrile solution containing 4.7% by weight of cyclohexanone, and 115 g of an acetonitrile solution containing 3.9% by weight of ammonia were separately fed (co-fed) into the reactor for 1 hour. The concentration of ammonia in the liquid phase of the reaction mixture varies in the range of 1.0 to 2.6% by weight relative to the liquid phase.

[0024] After the co-feed, the liquid phase of the reaction mixture was withdrawn and analyzed by gas chromatography. The conversion...

Embodiment 2

[0026] In a 1 L autoclave (reactor), 158.7 g of an acetonitrile solution containing 2.6% by weight of ammonia, 5.5 g of an n-decane solution containing 65% by weight of tert-butyl hydroperoxide and 5.0 g of Ti-MWW (prepared by the same method as described in Chemistry Letters, 2000, pp. 774-775), and the gas phase part in the reactor was replaced with nitrogen. After the reactor was sealed, the temperature in the reactor was raised to 110° C. with stirring. The pressure in the reactor was 0.5 MPa. Next, 10 g of an acetonitrile solution containing 4.7% by weight of cyclohexanone, and 115 g of an acetonitrile solution containing 3.8% by weight of ammonia were separately fed (co-fed) into the reactor for 1 hour. The concentration of ammonia in the liquid phase of the reaction mixture varies in the range of 1.0 to 2.6% by weight relative to the liquid phase.

[0027] After the co-feed, the liquid phase of the reaction mixture was withdrawn and analyzed by gas chromatography. Th...

Embodiment 3

[0029]In a 1 L autoclave (reactor), 158.8 g of ethanol solution containing 4.3% by weight of ammonia, 7.6 g of cumene solution containing 80% by weight of cumene hydroperoxide and 5.0 g of Ti-MWW (via prepared in the same manner as described in Chemistry Letters, 2000, pp. 774-775), and replaced the gas phase part of the reactor with nitrogen. After the reactor was sealed, the temperature in the reactor was raised to 110° C. with stirring. The pressure in the reactor was 0.5 MPa. Next, 10 g of an ethanol solution containing 4.7% by weight of cyclohexanone, and 115 g of an ethanol solution containing 3.8% by weight of ammonia were separately fed (co-fed) into the reactor for 1 hour. The concentration of ammonia in the liquid phase of the reaction mixture was varied in the range of 2.5 to 4.3% by weight relative to the liquid phase.

[0030] After the co-feed, the liquid phase of the reaction mixture was withdrawn and analyzed by gas chromatography. The conversion of cyclohex...

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PUM

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Abstract

The present invention provides a method for producing an oxime by carrying out an ammoximation reaction of a ketone with an organic peroxide and ammonia in a solvent in the presence of a titanosilicate, characterized in that the reaction is carried out by feeding the ketone and ammonia to a reactor in which the solvent, the titanosilicate and the organic peroxide are charged.

Description

technical field [0001] The present invention relates to a process for the preparation of oximes by the ammoximation reaction of ketones. Oximes can be used as starting materials for amides or lactams. Background technique [0002] The ammoximation reaction of ketones with hydrogen peroxide and ammonia in the presence of titanosilicate in a solvent is known in the art (JP 2006-169168 A, JP 2007-1952 A and JP 2007-238541 A) . However, hydrogen peroxide is not necessarily cost-effective. Therefore, a method of using an organic peroxide as a recyclable peroxide has been studied, but this method is not always satisfactory because the selectivity or yield of oxime is not stable for industrial production. Contents of the invention [0003] The present invention provides a process for the preparation of an oxime comprising: reacting a ketone with an organic peroxide and ammonia in a solvent in the presence of titanosilicate, wherein the ketone and ammonia are fed to a Reactors...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/04C07C251/44
CPCC07C2101/14C07C249/04C07C2601/14C07C251/44C07C249/08C07C251/32
Inventor 老川幸北村胜
Owner SUMITOMO CHEM CO LTD
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