Tert-octyl salicylaldoxime and synthetic method thereof

A technology of tert-octyl salicyl aldoxime and ter-octyl phenol is applied in the field of novel alkyl salicyl aldoxime and its synthesis, and achieves the effects of wide source of raw materials, low synthesis cost and good extraction performance

Inactive Publication Date: 2017-07-21
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis of tert-octyl salicylaldoxime with 8 carbon atoms in the R group has never been reported

Method used

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  • Tert-octyl salicylaldoxime and synthetic method thereof
  • Tert-octyl salicylaldoxime and synthetic method thereof
  • Tert-octyl salicylaldoxime and synthetic method thereof

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Experimental program
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Effect test

Embodiment 1

[0016] The control synthesis process conditions are as follows: the molar ratio n (magnesium: p-tertoctylphenol) is 0.55:1, the salt-forming reaction time is controlled at 110 minutes, and the salt-forming reaction temperature is controlled at reflux reaction at 63°C; the molar ratio n (more Polyoxymethylene: p-tetraoctylphenol) is 2.40:1, the acylation temperature is controlled at 107° C. with an oil bath, and the acylation reaction time is controlled at 150 minutes; the mol ratio n (hydroxylamine hydrochloride: p-teroctylphenol) is 1.50:1, select the oximation reaction temperature between 45-50°C, control the oil bath temperature at 47°C, and control the oximation reaction time at 210 minutes. Add 2 times of toluene when the methanol-toluene azeotrope is distilled out in the salt formation reaction, and add 5 mL of toluene 3 times during the acylation reaction, with an interval of 2 minutes between each time. After this step, the crude product of tert-octyl salicylaldoxime c...

Embodiment 2

[0022] The control synthesis process condition is as follows: the molar ratio n (magnesium: p-tertoctylphenol) is 0.50: 1, the salt-forming reaction time is controlled at 110 minutes, and the salt-forming reaction temperature is controlled at reflux reaction when 63 ℃; Polyoxymethylene: p-tert-octylphenol) is 2.40: 1, the acylation temperature is controlled at 107 ℃ with an oil bath, and the acylation reaction time is controlled at 150 minutes; the mol ratio n (hydroxylamine hydrochloride: p-tert-octylphenol) is 1.50:1, select the oximation reaction temperature between 45-50°C, control the oil bath temperature at 47°C, and control the oximation reaction time at 210 minutes. Add 2 times of toluene when the methanol-toluene azeotrope is distilled out in the salt formation reaction, and add 5 mL of toluene 3 times during the acylation reaction, with an interval of 2 minutes between each time. After this step, the crude product of tert-octyl salicylaldoxime can be obtained, which ...

Embodiment 3

[0024] The control synthesis process condition is as follows: the molar ratio n (magnesium: p-tertoctylphenol) is 0.50: 1, the salt-forming reaction time is controlled at 90 minutes, and the salt-forming reaction temperature is controlled at reflux reaction when 63 ℃; Polyoxymethylene: p-tert-octylphenol) is 2.40: 1, the acylation temperature is controlled at 107 ℃ with an oil bath, and the acylation reaction time is controlled at 150 minutes; the mol ratio n (hydroxylamine hydrochloride: p-tert-octylphenol) is 1.50:1, select the oximation reaction temperature between 45-50°C, control the oil bath temperature at 47°C, and control the oximation reaction time at 210 minutes. Add 2 times of toluene when the methanol-toluene azeotrope is distilled out in the salt formation reaction, and add 5 mL of toluene 3 times during the acylation reaction, with an interval of 2 minutes between each time. After this step, the crude product of tert-octyl salicylaldoxime can be obtained, which i...

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Abstract

The invention relates to tert-octyl salicylaldoxime and a synthetic method thereof. The synthetic process conditions are as follows: the molar ratio of magnesium: p-tert-octyl phenol is 0.55:1, the salt forming reaction time is 110 minutes and the salt forming reaction temperature is 63 DEG C; the molar ratio of paraformaldehyde: p-tert-octyl phenol is 2.4:1, the acylation temperature is controlled to be 107 DEG C by oil bath, and the time is 150 minutes; the molar ratio of hydroxylamine hydrochloride: p-tert-octyl phenol is 1.5:1, the oximation reaction temperature is between 45 DEG C and 50 DEG C, the boil bath temperature is 47 DEG C, and the time is 210 minutes; adding methylbenzene for two times while methanol-methylbenzene azeotrope is distilled in the salt forming reaction, and adding the methylbenzene for three times in the acylation reaction, wherein 5 ml of the methylbenzene is added every time, and the time interval is 2 minutes; to obtain a tert-octyl salicylaldoxime coarse product, acidifying, distilling in the reduced pressure and washing by petroleum ether, to obtain the tert-octyl salicylaldoxime. Compared with other common copper extraction agents, the tert-octyl salicylaldoxime has the advantages of low synthesis cost and extensive raw material source.

Description

technical field [0001] The invention relates to a novel alkyl salicylaldoxime and its synthesis technology, in particular to a tert-octyl salicylaldoxime and its synthesis method. Background technique [0002] Alkyl salicylaldoxime has a very strong chelating effect on copper ions and is often used as an extractant in hydrometallurgical processes. The structural change of the R group on the para-position of the benzene ring in the alkyl salicylaldoxime will make the extractant have different hydrophobicity and steric hindrance effect, which will affect the extraction performance of the extractant on copper ions. Many straight-chain alkanes alkyl salicylaldoximes with different numbers of carbon atoms have been reported, including straight-chain alkanes with 9, 10 and 12 carbon atoms. However, the synthesis of tert-octyl salicylaldoxime with 8 carbon atoms in the R group has never been reported. Contents of the invention [0003] The object of the present invention is to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/48C07C249/12
CPCC07C249/08C07C37/66C07C45/45C07C249/12C07C251/48
Inventor 李立清肖友军陈喜蓉李敏肖焱尹王义安文娟
Owner JIANGXI UNIV OF SCI & TECH
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