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Synthesis method for glycocyamine with high purity and high yield

A synthesis method and technology of guanidinoacetic acid, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of unsuitability for large-scale industrial production, long synthesis route, poor quality, etc., and achieve high economy and Environmental protection, short production cycle, less waste

Inactive Publication Date: 2016-04-20
ZHEJIANG ESIGMA BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a long synthetic route, time-consuming, low yield, poor quality, and the problem of excessive bromoethane and ethanol recovery, which is not suitable for large-scale industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 25.5g (0.34mol) of glycine and 28.1g of water into a 250mL four-necked flask equipped with a reflux condenser, dropping funnel and thermometer, stir to dissolve, add liquid ammonia to adjust the pH to 10.0, raise the temperature to 55°C, and slowly add 28g (0.33mol) of 50% cyanamide aqueous solution, stirred and reacted for 3h, suction filtered, and washed with the filtrate; in another reaction kettle, add crude guanidinoacetic acid and 2 times the mass of DMF, heat to 35°C and stir for 0.5h, then cool to 0°C, after suction filtration, washing the filter cake with DMF, and drying, finally obtained 37.33 g of guanidinoacetic acid with a yield of 93.2% and a content of 99.3%.

Embodiment 2

[0020] Add 26.2g (0.35mol) of glycine into a 250mL four-necked flask equipped with a reflux condenser, dropping funnel and thermometer, and 34.1g of the filtrate obtained from the first filtration in Example 1, stir to dissolve, and add liquid ammonia to adjust the pH to 10.3 , the temperature was raised to 57°C, and 28g (0.33mol) of 50% cyanamide aqueous solution was slowly added dropwise, stirred and reacted for 2h, filtered with suction, and the filter cake was washed with the filtrate. Add crude guanidinoacetic acid and 3 times the mass of DMF into another reaction kettle, heat to 37°C and stir for 0.5h, then cool to 0°C, filter with suction, wash the filter cake with DMF, and dry to obtain guanidinoethyl, 39.26g, The yield is 95.4%, and the content is 99.5%.

Embodiment 3

[0022] Add 27.0g (0.36mol) of glycine and 40.5g of water into a 250mL four-neck flask equipped with a reflux condenser, dropping funnel and thermometer, stir to dissolve, add liquid ammonia to adjust the pH to 11, raise the temperature to 60°C, and slowly add 27.5 g (0.327 mol) of 50% cyanamide aqueous solution was stirred for 4 hours, filtered with suction, and washed with the filtrate. Add crude guanidinoacetic acid and 4 times the mass of DMF into another reaction kettle, heat to 40°C and stir for 0.5h, then cool to 0°C, filter with suction, wash the filter cake with DMF, and dry to obtain 39.93g of guanidinoacetic acid. The rate is 94.6%, and the content is 99.8%.

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Abstract

The invention discloses a synthesis method for glycocyamine with high purity and high yield. The synthesis method comprises the following steps: (1) adding glycine and a solvent into a reaction vessel, stirring at room temperature till glycine is dissolved completely, and adding liquid ammonia to adjust the pH value of the solution to be 10 to 11; (2) heating the mixed solution obtained in the step (1) to 55 to 60 DEG C, adding 50% hydrogen cyanamide aqueous solution into the reaction vessel slowly, stirring for 2 to 4 hours for reaction, carrying out vacuum suction filtration after the reaction is finished, and washing filter cake with filtrate to obtain a crude product of glycocyamine; (3) adding the crude product of glycocyamine obtained in the step (2) and DMF into another reaction vessel, heating to 30 to 40 DEG C, stirring for 0.5 hour, cooling to 0 DEG C, carrying out suction filtration, washing filter cake with DMF, and drying to obtain glycocyamine. The preparation method provided by the invention is simple in technology, short in production period, mild in reaction conditions, less in three wastes, high in product purity and yield, and relatively high in economical efficiency and environmental friendliness, thereby being suitable for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for synthesizing guanidinoacetic acid with high purity and high yield. Background technique [0002] Guanidinoacetic acid is white or slightly yellow crystalline powder, soluble in water, very slightly soluble in ethanol and ether. Guanidinoacetic acid is mainly used as an intermediate in pharmaceutical organic synthesis, and can also be used as a food and feed additive. It plays an important role in improving production performance, improving meat quality and promoting energy metabolism. In addition, it can prevent bacterial infection, enhance animal immune function, reduce The effect of heat stress on animals, thereby reducing the mortality of animals in high temperature environments. [0003] According to relevant literature reports, the main production process of guanidinoacetic acid is: mix thiourea, ethyl bromide and absolute ethanol, and warm in a water...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C277/08C07C279/14
CPCC07C277/08
Inventor 闻鸣徐天华吴江波何奇雷
Owner ZHEJIANG ESIGMA BIOTECH CO LTD
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