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Synthetic method for acetohydroxamic acid

A technology for the synthesis of acetylhydroxamic acid and its method, which is applied in the field of synthesizing acetylhydroxamic acid, can solve the problems of no significant improvement in yield and purity, and achieve the effects of easy industrialization, easy availability of raw materials, and simple process

Active Publication Date: 2015-12-16
BEIJING SUNPU BIOCHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The collection of raw materials and the control of temperature in the production process in the above production processes have all met the cost control and safety requirements, but the yield and purity issues have not been significantly improved, and there is no solution to the core issues such as yield and purity. come up with effective solutions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Acetohydroxamic acid was synthesized from the mixture solution of sodium ethoxide and ethanol as catalyst and hydroxylamine sulfate and ethyl acetate as raw materials.

[0042] Add hydroxylamine sulfate 16.4g (0.1mol) in the reactor, room temperature drips the ethanolic solution 153.0g of 20% sodium ethylate, wherein sodium ethylate and hydroxylamine sulfate mol ratio are 4.5:1, stir, dropwise for about 1h, obtain Continue to add 20.3g (0.23mol) of ethyl acetate dropwise to the precipitated mixed solution. After about 1 hour, the reaction is completed for 2 hours. The reaction temperature is maintained at 25°C to 30°C. End point pH = 6, suction filtration and concentration to obtain about 10ml of concentrated solution, crystallize with 100ml of mixed solvent of chloroform and ethanol at a volume ratio of 8:1, and obtain 14.8g of needle-like crystal acetohydroxamic acid with a yield of 98.6%, continue to use The volume ratio of chloroform and ethanol was 5:1 and recrysta...

Embodiment 2

[0044]16.4 g (0.1 mol) of hydroxylamine sulfate was added to the reactor, and 68.0 g of 20% sodium ethylate ethanol solution was added dropwise at room temperature, wherein the molar ratio of sodium ethylate to hydroxylamine sulfate was 2:1, stirred, and the dropwise addition was completed in about 0.5 h to obtain Continue to add 17.6g (0.2mol) of ethyl acetate dropwise to the mixed solution with precipitation, and complete the reaction for about 1 hour. The reaction temperature is maintained at 25°C for 1 hour. =6, suction filtration and concentration to obtain about 10 ml of concentrated solution, crystallize with 60 ml of mixed solvent of chloroform and ethanol at a volume ratio of 9:1 to obtain 14.6 g of acicular crystal acetylhydroxamic acid, yield 97.1%.

Embodiment 3

[0046] Add hydroxylamine sulfate 16.4g (0.1mol) in the reactor, room temperature drips the ethanol solution 85.0g of 40% sodium ethylate, wherein sodium ethylate and hydroxylamine sulfate mol ratio are 5:1, stir, about 1h dropwise, obtain Continue to add 22.0g (0.25mol) of ethyl acetate dropwise to the precipitated mixed solution for about 1 hour, react for 2 hours, keep the reaction temperature at about 25°C, and after the reaction is completed, slowly add concentrated sulfuric acid to adjust to the final pH while continuing to stir = 6, suction filtration and concentration to obtain about 10 ml of concentrated solution, crystallize with 120 ml of mixed solvent of chloroform and ethanol at a volume ratio of 6:1 to obtain 14.5 g of needle-like crystals of acetohydroxamic acid, with a yield of 96.6%.

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Abstract

The invention relates to a synthetic method for acetohydroxamic acid. The method synthesizes the acetohydroxamic acid with hydroxylamine sulfate and ethyl acetate as raw materials and with an ethanol solution of sodium ethoxide as a catalyst. Compared with a traditional synthetic method (e.g., using sodium hydroxide as the catalyst), the synthetic method provided by the invention has the advantages of simple and convenient process, easily-available raw materials which are bulk chemical materials, low cost, high yield and facilitation to industrial popularization.

Description

technical field [0001] The invention relates to a method for synthesizing acetyl hydroxamic acid. Background technique [0002] Acetohydroxamic acid, also known as acetohydroxamic acid, is widely used in medicine, animal husbandry, agriculture, environmental protection, metallurgy, etc. In the feed industry, it is used as a rumen microbial urease inhibitor for ruminant feed additives; in medicine, it is a competitive inhibitor of urease, and the trade name is Junshitong; in the metallurgical industry, it is used as a chelating agent and extractant for the extraction of metal ions and identification etc. [0003] At present, most of the synthesis methods of acetylhydroxamic acid are chemical synthesis. Su Lanhui and Jiang Xiangyang used ethyl acetate and hydroxylamine hydrochloride to react in a system using methanol as a solvent in the "Research on the Synthesis Process of Acetohydroxamic Acid" (China Feed). To prepare acetohydroxamic acid, use hydroxylamine hydrochloride ...

Claims

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Application Information

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IPC IPC(8): C07C259/06
Inventor 裴双秀胡冬琴潘咏梅蒙雪艳胡文静
Owner BEIJING SUNPU BIOCHEM TECH
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