Continuous production process method of hydroxyguanidine sulfate

A technology of hydroxyguanidine sulfate and production process, which is applied in the field of preparation process of hydroxyguanidine sulfate, can solve problems such as inability to directly react in one step, unfavorable continuous reaction, long reaction time, etc., achieve automatic continuous production, shorten reaction time, The effect of low raw material cost

Active Publication Date: 2021-11-26
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method needs to mix hydroxylamine sulfate and barium hydroxide first, filter out the precipitate, and then react the filtrate with O-methylisourea sulfate, which cannot be directly reacted in one step, and is not conducive to continuous reaction
At the same time, the reaction time is too long and the yield is low

Method used

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  • Continuous production process method of hydroxyguanidine sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Through the plunger pump, the mass fraction of 30% hydroxyguanidine sulfate aqueous solution and the mass fraction of 50% cyanamide aqueous solution are passed into the microchannel reactor at a mixing ratio of 1:1 (v / v) for condensation reaction, and the reaction temperature is 5 ° C. The reaction time is 300s, the reaction pressure is 1.2Mpa, and the reaction feed liquid containing hydroxyguanidine sulfate obtained after the reaction is completed. It is pumped into the concentrated crystallization kettle through a high-pressure plunger pump for concentration under reduced pressure, and ethanol is passed through to cool down and crystallize. The volume ratio of the ethanol solution and the concentrated solution is 1:5. Finally, centrifuge filtration and drying to obtain hydroxyguanidine sulfate, and the calculated product yield is 72.1%.

Embodiment 2-3

[0030] The difference from the production method in Example 1 is that the mass fraction of the cyanamide aqueous solution used in this example is 70% (Example 2) and 30% (Example 3).

Embodiment 4-5

[0032] The difference from Example 1 is that in this example, the reaction temperature is 0°C (Example 4) and 10°C (Example 5).

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PUM

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Abstract

The invention discloses a continuous production process method of hydroxyguanidine sulfate, and belongs to the field of organic synthesis. According to the method, cyanamide and hydroxylamine sulfate serve as raw materials, a condensation reaction is conducted through the microchannel reactor, the reaction liquid containing hydroxyguanidine sulfate is obtained, the preparation method is simple, the reaction time is short, and the reaction efficiency is high. The final product has high purity, impurities are easy to remove, and the product yield reaches 70-80%. The whole system achieves automatic continuous production, is high in resource utilization rate, saves energy and reduces consumption, the obtained mixed solution containing hydroxyguanidine sulfate is concentrated, cooled and crystallized to obtain hydroxyguanidine sulfate, and continuous production in the process from feeding to crystallization is achieved.

Description

technical field [0001] The invention relates to a preparation process of hydroxyguanidine sulfate, which belongs to the field of organic synthesis. Background technique [0002] Hydroxyguanidine sulfate is an antimetabolite antineoplastic drug, which acts on the S phase of the cell cycle, interferes with DNA synthesis by inhibiting nucleotide reductase, and acts on late hematopoietic cells. As an anti-tumor drug, it is often used in combination with other types of anti-tumor drugs to treat cancer in clinical practice. [0003] There are following several methods for preparing hydroxyguanidine sulfate in the prior art at present: (1) use cyanamide and hydroxylamine as raw material and add sulfate to obtain product hydroxyguanidine sulfate after condensation reaction, and total yield is 49%, and atom utilization rate High, cheap raw materials. However, the raw material cyanamide self-polymerizes to form dicyandiamide and even polymers: cyanamide and hydration form urea, etc....

Claims

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Application Information

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IPC IPC(8): C07C277/08C07C279/00B01J19/00
CPCC07C277/08B01J19/0093C07C279/00
Inventor 董航高岩张华
Owner DALIAN UNIV OF TECH
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