A kind of synthetic method of stable isotope labeling dicyandiamide

A stable isotope and isotope labeling technology, which is applied in the fields of isotope introduction into organic compounds, organic chemistry methods, chemical instruments and methods, etc., can solve the problem that the device is difficult to meet the requirements of isotope synthesis, the introduction of isotope-labeled elements, and is not suitable for the synthesis of stable isotope-labeled compounds. and other problems, to achieve the effect of good economy and use value, stable marking position, and good promotion prospects

Active Publication Date: 2017-02-01
SHANGHAI RES INST OF CHEM IND
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  • Abstract
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Problems solved by technology

[0008] At present, the industrial synthesis methods of dicyandiamide mainly include calcium cyanamide method, urea method, etc., but the devices involved in these synthesis processes are difficult to meet the requirements of isotope synthesis, and it is difficult to introduce isotope-labeled elements, so it is not suitable for stable isotope-labeled compounds. Synthesis
And there is no relevant bibliographical report both at home and abroad about the synthetic technology of stable isotope labeling dicyandiamide

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  • A kind of synthetic method of stable isotope labeling dicyandiamide
  • A kind of synthetic method of stable isotope labeling dicyandiamide
  • A kind of synthetic method of stable isotope labeling dicyandiamide

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Take 6.4g of calcium carbide and 0.1g of calcium chloride and mix them evenly and add them into the reactor, vacuumize until the pressure is -0.1MPa, put the reactor into a tube furnace and start heating, and continue pumping when the temperature rises to 800°C Vacuum to -0.1MPa, then open 15 N 2 Gas valve, slowly introduce 1.5L gas, keep the temperature and react for 1h. After the reaction is over, the stable isotope labeled calcium cyanamide- 15 N 2 .

[0041] The calcium cyanamide obtained by the above reaction- 15 N 2Mix with distilled water at a mass ratio of 1:4.5, hydrolyze at 25°C, and start to introduce carbon dioxide gas after 2 hours until the mixed liquid is weakly alkaline, add 0.02g of sodium hydroxide solid to the mixed liquid after suction filtration, and stir the reaction at 50°C 6h, the cooling crystallization at the end of the reaction, to obtain 0.89g target product stable isotope labeled dicyandiamide- 15 N 4 . by access 15 N 2 Gas meter,...

Embodiment 2

[0043] Take 5.6g calcium oxide, 12.4g stable isotope labeled urea- 15 N 2 , 0.18g of silicon dioxide mixed evenly into the reactor, heated to 260 ° C for 2 hours, after the reaction was completed and calcined at 700 ° C for several hours, the stable isotope labeled calcium cyanamide- 15 N 2 .

[0044] The calcium cyanamide obtained by the above reaction- 15 N 2 Mix with distilled water at a mass ratio of 1:5.5, hydrolyze at 10°C, and start to introduce carbon dioxide gas after 3 hours until the mixed solution is weakly alkaline, add 0.06g of potassium hydroxide solid to the mixed solution after suction filtration, and stir the reaction at 60°C 4h, the reaction finishes cooling crystallization, obtains 1.6g target product stable isotope labeled dicyandiamide- 15 N 4 . With urea- 15 N 2 The total yield was 18.4%. The product was detected by liquid chromatography and mass spectrometry. The purity was 99.3%, and the abundance was 99.1%. 15 N.

Embodiment 3

[0046] Take 6.4g of calcium carbide and 0.18g of calcium chloride and mix them evenly and add them into the reactor, vacuumize until the pressure is -0.1MPa, put the reactor into a tube furnace and start heating, and continue pumping when the temperature rises to 1200°C Vacuum to -0.1MPa, then open 15 N 2 Gas valve, slowly introduce 1.5L gas, keep the temperature for 2h. After the reaction is over, the stable isotope labeled calcium cyanamide- 15 N 2 .

[0047] The calcium cyanamide obtained by the above reaction- 15 N 2 Mix with distilled water at a mass ratio of 1:3.5, hydrolyze at 35°C, and start to introduce carbon dioxide gas after 4.5 hours until the mixed liquid is weakly alkaline, add 0.01g of sodium ethoxide solid to the mixed liquid after suction filtration, and stir the reaction at 70°C 3h, the cooling crystallization after reaction finishes, obtains 1.49g target product stable isotope labeled dicyandiamide- 15 N 4 . by access 15 N 2 Gas meter, the total ...

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Abstract

The invention relates to a synthesis method of stable isotope labeling cyanoguanidine. Specifically, the method comprises the following steps: by virtue of an organic chemical synthesis method, with stable isotope labeling nitrogen or urea as an isotope labeling precursor, reacting with calcium carbide or calcium oxide under the action of a catalyst to obtain calcium cyanamide; and hydrolyzing, decalcifying, and polymerizing to obtain the stable isotope labeling cyanoguanidine. Compared with the prior art, according to the stable isotope labeling cyanoguanidine provided by the invention, the isotope labeling position is stable; dilution of isotope abundance is avoided; the isotope abundance is more than 99.0% atom15N; the chemical purity is equal to or greater than 99.0% after the product is purified; and the requirements of residue detection in the field of food safety can be fully met.

Description

technical field [0001] The invention relates to a synthesis method of a stable isotope internal standard substance, in particular to a synthesis method of a stable isotope labeled dicyandiamide. Background technique [0002] Dicyandiamide, also known as cyanoguanidine and dicyandiamide, is soluble in water, ethanol and acetonitrile, and is mainly used as a fertilizer and other fine chemical intermediates. Dicyandiamide has certain toxicity. The toxicity test on mice showed that 16 hours after administration of the highest dose group, the mice began to appear uneasy, jumping, and short of breath, and then died within tens of minutes. New Zealand farmers use dicyandiamide in pastures mainly to prevent nitrates from flowing into rivers and causing pollution, but due to the transmission of biological chains, there are also dicyandiamide residues in milk. In January 2013, the news about the detection of dicyandiamide residues in some New Zealand milk powder aroused widespread co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C279/28C07C277/08C07B59/00
Inventor 吕靖杨维成罗勇杨超盛立彦李美华
Owner SHANGHAI RES INST OF CHEM IND
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