Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF4 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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).

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C277/08C07C279/00B01J19/00
CPCC07C277/08B01J19/0093C07C279/00
Inventor 董航高岩张华
Owner DALIAN UNIV OF TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com