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Preparation technology of caprylhydroxamic acid

A technology for the preparation of caprylyl hydroxamic acid, which is applied in the field of preparation of caprylyl hydroxamic acid, can solve the problems of low yield, achieve the effects of improving yield and purity, wide temperature range, and improving production efficiency

Active Publication Date: 2020-02-28
菏泽新东方日化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] However, the above-mentioned preparation method generally has the problem of low yield. The yield in the Chinese patent application whose publication number is CN106588697A is the highest, but only 84%. How to further improve the yield of octanoylhydroxamic acid is directly related to the profit of the enterprise , is also the focus of current research and development

Method used

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  • Preparation technology of caprylhydroxamic acid
  • Preparation technology of caprylhydroxamic acid
  • Preparation technology of caprylhydroxamic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A kind of preparation technology of caprylyl hydroxamic acid, the mol ratio of each material that adopts is as follows:

[0042] The molar ratio of compound 2 to composite catalyst is 1:0.014;

[0043] In the composite catalyst, the mol ratio of sodium acetate to sodium carbonate is 1:0.4;

[0044] The molar ratio of compound 2 to hydroxylamine is 1:1.003;

[0045] The molar ratio of compound 1 to ethanol is 1:1.1,

[0046] Specifically, the following steps are included:

[0047] (a) preparation of n-octanoic acid ethyl ester

[0048] Mix 14.421g (0.1mol, 1.0eq) of compound 1 and 5.068g (0.11mol, 1.1eq) of ethanol, add 1mL of sulfuric acid, heat to reflux for 5 hours, neutralize with sodium hydroxide solution, and distill under reduced pressure to obtain 16.167g Colorless liquid product, based on compound 2, the purity of the colorless liquid product is 99.2%, and the yield is 93.1%;

[0049] (b) Preparation of Caprylyl Hydroxamic Acid

[0050] Mix 6.169g (0.09337...

Embodiment 2

[0052] A kind of preparation technology of caprylyl hydroxamic acid, the mol ratio of each material that adopts is as follows:

[0053] The molar ratio of compound 2 to composite catalyst is 1:0.03;

[0054] In the composite catalyst, the mol ratio of sodium acetate to sodium carbonate is 1:0.5;

[0055] The molar ratio of compound 2 to hydroxylamine is 1:1.004;

[0056] The molar ratio of compound 1 to ethanol is 1:1.2,

[0057] Specifically, the following steps are included:

[0058] (a) preparation of n-octanoic acid ethyl ester

[0059] Mix 14.421g (0.1mol, 1.0eq) of compound 1 and 5.528g (0.12mol, 1.2eq) of ethanol, add 1mL of sulfuric acid, heat to reflux for 5 hours, neutralize with sodium hydroxide solution, and distill under reduced pressure to obtain 16.294g Colorless liquid product, based on compound 2, the purity of the colorless liquid product is 99.8%, and the yield is 94.4%;

[0060] (b) Preparation of Caprylyl Hydroxamic Acid

[0061] Mix 6.261g (0.094778...

Embodiment 3

[0063] A kind of preparation technology of caprylyl hydroxamic acid, the mol ratio of each material that adopts is as follows:

[0064] The molar ratio of compound 2 to composite catalyst is 1:0.036;

[0065] In the composite catalyst, the mol ratio of sodium acetate to sodium carbonate is 1:0.6;

[0066] The molar ratio of compound 2 to hydroxylamine is 1:1.005;

[0067] The molar ratio of compound 1 to ethanol is 1:1.3,

[0068] Specifically, the following steps are included:

[0069] (a) preparation of n-octanoic acid ethyl ester

[0070] Mix 14.421g (0.1mol, 1.0eq) of compound 1 and 5.989g (0.13mol, 1.3eq) of ethanol, add 1mL of sulfuric acid, heat to reflux for 5 hours, neutralize with sodium hydroxide solution, and distill under reduced pressure to obtain 16.395g Colorless liquid product, based on compound 2, the purity of the colorless liquid product is 99.5%, and the yield is 94.7%;

[0071] (b) Preparation of Caprylyl Hydroxamic Acid

[0072] Mix 6.287g (0.09517...

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Abstract

The invention discloses a preparation technology of caprylhydroxamic acid, and belongs to the technical field of chemical synthesis. The preparation technology comprises following steps: (a) preparingethyl n-octanoate from n-octanoic acid and ethanol under the catalytic action of sulfuric acid under a heating reflux condition; and (b) under the action of a composite catalyst, carrying out hydroxyl-oximation reactions between ethyl n-octanoate and hydroxylamine for 1.5 to 4 hours at a temperature of 30 to 60 DEG C to obtain caprylhydroxamic acid; wherein the composite catalyst comprises sodiumacetate and sodium carbonate, the mole ratio of ethyl n-octanoic to the composite catalyst is 1:0.01 to 1:0.03, and the mole ratio of sodium acetate to sodium carbonate of the composite catalyst is 1:0.4 to 1:0.6. By picking and using the composite catalyst, the yield and purity of caprylhydroxamic acid are both increased, and the reaction time is shortened.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation process of caprylyl hydroxamic acid. Background technique [0002] Capryl hydroxamic acid, that is, capryl hydroxamic acid, INCI name: Caprylhydroxamic Acid, referred to as CHA, molecular formula: C 8 h 17 NO 2 , molecular weight: 159.23, CAS registration number: 7377-03-9, white or off-white powder, the structural formula is as follows: [0003] [0004] Caprylyl hydroxamic acid is an organic acid that can maintain a non-ionized state from acidic to neutral. It has high-efficiency chelation, can inhibit the active elements required by mold, and limit the environment required for microbial growth. It is an ideal antibacterial agent , Widely used in cosmetics, medicine and fine chemical industry. [0005] About the preparation of octanoyl hydroxamic acid disclosed in the prior art, brief introduction is as follows: [0006] The Chinese patent appli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C259/06B01J31/26
CPCC07C259/06B01J31/26
Inventor 薛天辉陈晓辉陈坤秦莉锦
Owner 菏泽新东方日化科技有限公司
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