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Preparation method of amino hydroxyurea

A technology of semicarbazide and urethane, which is applied in the field of preparation of semicarbazide, can solve the problems of no practical value in large-scale production, low yield, and high cost, and achieve low production cost, high reaction yield, and simple operation Effect

Active Publication Date: 2022-05-06
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing preparation method of hydroxysemicarbazide requires the use of high-cost and highly toxic phenoxychloride as a raw material, and adopts a two-step synthesis method at the same time, and the yield is low, which does not have practical value for large-scale production

Method used

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  • Preparation method of amino hydroxyurea
  • Preparation method of amino hydroxyurea
  • Preparation method of amino hydroxyurea

Examples

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preparation example Construction

[0025] refer to Figure 1 to Figure 3 , the present disclosure provides a preparation method of hydroxysemicarbazide, the preparation method may include: under urethane exchange conditions and in the presence of an acid-binding agent, contacting a substance of formula A and a substance of formula B in a solvent to obtain materials after contact.

[0026]

[0027] In the present invention, in the substance of formula A, R is any one of the following substituents:

[0028]

[0029] The substance of formula B is at least one of hydroxylamine, hydroxylamine hydrochloride, hydroxylamine sulfate, hydroxylamine phosphate, hydroxylamine sulfonate and hydroxylamine nitrate. The substance of formula A is preferably at least one of the The substance of formula B is preferably at least one of hydroxylamine, hydroxylamine hydrochloride and hydroxylamine sulfate.

[0030] Optionally, the molar ratio of the substance of formula A to the substance of formula B is 1:1-3.

[0031] A...

Embodiment 1

[0044] Under urethane exchange conditions and in the presence of an acid-binding agent (sodium hydroxide), a substance of formula A (ethyl carbazate) and a substance of formula B (hydroxylamine) are contacted in a solvent (ethanol) to obtain contact After the material; the molar ratio of the substance of the formula A and the substance of the formula B is 1:2.4; the urethane exchange conditions include: the temperature is 10 ° C, the time is 24h; relative to each mole of the formula For the substance of A, the amount of the solvent used is 0.79 L; the amount of the acid-binding agent used is 1.2 mol.

[0045] The contacted materials were subjected to reduced-pressure rotary evaporation and first drying to obtain a crude product; the temperature of the reduced-pressure rotary evaporation was 60° C.; the temperature of the first drying was 80° C. for 16 hours.

[0046] Mix and re-dissolve the crude product with ethanol and water, then carry out recrystallization, filtration and ...

Embodiment 2

[0048] Under urethane exchange conditions and in the presence of an acid-binding agent (sodium carbonate), a substance of formula A (methyl carbazate) and a substance of formula B (hydroxylamine hydrochloride) are contacted in a solvent (ethanol) to obtain contact After the material; the molar ratio of the substance of the formula A and the substance of the formula B is 1:1.2; the urethane exchange conditions include: room temperature, the time is 48h; relative to the substance of the formula A per mole , the amount of the solvent is 0.833L; the amount of the acid-binding agent is 1.198mol.

[0049] The contacted materials were subjected to reduced-pressure rotary evaporation and first drying to obtain a crude product; the temperature of the reduced-pressure rotary evaporation was 65° C.; the temperature of the first drying was 80° C. for 16 hours.

[0050] Mix and re-dissolve the crude product with ethanol and water, then carry out recrystallization, filtration and second dry...

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Abstract

The invention relates to a preparation method of amino hydroxyurea, which comprises the following steps: under the condition of ammonia ester exchange and in the presence of an acid-binding agent, contacting a substance shown in a formula A with a substance shown in a formula B in a solvent to obtain a contacted material, carrying out reduced pressure rotary evaporation and first drying on the contacted material to obtain a crude product; mixing the crude product with ethanol and water, re-dissolving, recrystallizing, filtering and secondarily drying; and carrying out second drying to obtain the target product amino hydroxyurea. The method for one-step preparation of amino hydroxyurea through ammonia-ester exchange provided by the invention has the advantages of short synthetic route, cheap and easily available raw materials, high process safety, simple operation, low production cost and high reaction yield, and is suitable for industrial production.

Description

technical field [0001] The disclosure relates to the technical field of organic synthesis, in particular to a preparation method of hydroxysemicarbazide. Background technique [0002] The chemical name of hydroxysemicarbazide is N-hydroxy-1-hydrazinecarboxamide, the English name is N-hydroxy-1-hydrazinecarboxamide; CAS number: 21520-79-6, molecular formula: CH 5 N 3 o 2 , molecular weight: 91.07. [0003] Semicarbazide can quickly react with Pu(Ⅳ) and Np(Ⅵ). Technetium has no interference with this process, and the reaction product is easily destroyed. At the same time, it can be used alone as a reducing stripping agent without supporting reducing agent, which can be eliminated in the process Technetium washing process. Therefore, hydroxysemicarbazide has a good application prospect in the Purex process. [0004] The existing preparation method of hydroxysemicarbazide requires the use of high-cost and highly toxic phenoxychloride as a raw material, and adopts a two-step...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C281/06
CPCC07C281/06Y02A50/30
Inventor 欧阳应根肖松涛
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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