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Synthesis method of pyrimidine aminoethyl methacrylate compound

The technology of pyrimidine aminoethyl methacrylate and isocyanoethyl methacrylate is applied in the field of synthesis of pyrimidine aminoethyl methacrylate compounds, and can solve the problems of environmental pollution, low yield and purity of finished products, and the like, Achieve the effect of ensuring purity, improving yield, and avoiding insufficient reaction

Inactive Publication Date: 2021-11-30
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] And its synthetic method of 2-[[[(1,6-dihydro-4-methyl-6-oxo-2-pyrimidinyl) amino] carbonyl] amino] ethyl methacrylate on the market is relatively complicated, Therefore cause the yield and the purity of its finished product to be all low, can use heavy metal to catalyze and easily pollute the environment simultaneously in part synthesis method, propose the synthetic method of pyrimidine amino ethyl methacrylate compound for this reason

Method used

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  • Synthesis method of pyrimidine aminoethyl methacrylate compound
  • Synthesis method of pyrimidine aminoethyl methacrylate compound
  • Synthesis method of pyrimidine aminoethyl methacrylate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The synthetic method of pyrimidine aminoethyl methacrylate compound, its synthetic steps are as follows:

[0024] Take 40mL of dimethyl sulfoxide and add it to the reaction flask, heat to 135°C, add 8.0g (0.064mol) of 2-amino-4-hydroxy-6-methylpyrimidine and stir to dissolve, after complete dissolution, move to 25°C Rapidly cool down to 25°C in a water bath environment, then quickly add 11.0g (0.071mol) isocyanoethyl methacrylate, and maintain 25°C for addition reaction for 6 hours. During the reaction process, the reaction system is always maintained at 25°C, which can inhibit It polymerizes violently, producing by-products. After the addition reaction was completed, it was vacuum filtered and washed three times with excess acetone, and the resulting white solid was dried in vacuo to obtain 17.65 g of methacrylic acid 2-[[[(1,6-dihydro-4-methyl-6 -Oxo-2-pyrimidinyl)amino]carbonyl]amino]ethyl ester, yield 98.39%, purity 99.5%, specific chemical reaction formula is as f...

Embodiment 2

[0028] The synthetic method of pyrimidine aminoethyl methacrylate compound, its synthetic steps are as follows:

[0029] Take 64mL of dimethyl sulfoxide and add it to the reaction flask, heat to 130°C, add 8.0g (0.064mol) of 2-amino-4-hydroxy-6-methylpyrimidine and stir to dissolve, after complete dissolution, move to 20°C Rapidly cool down to 20°C in a water bath environment, then quickly add 12.9g (0.083mol) isocyanoethyl methacrylate, maintain 20°C for addition reaction for 8 hours, keep the reaction system at 20°C during the reaction process, which can inhibit It polymerizes violently, producing by-products. After the addition reaction was completed, it was vacuum filtered and washed three times with excess acetone, and the resulting white solid was dried in vacuo to obtain 17.68 g of methacrylic acid 2-[[[(1,6-dihydro-4-methyl-6 -Oxo-2-pyrimidinyl)amino]carbonyl]amino]ethyl ester, yield 98.56%, purity 99.6%.

Embodiment 3

[0031] The synthetic method of pyrimidine aminoethyl methacrylate compound, its synthetic steps are as follows:

[0032] Take 50mL of dimethyl sulfoxide and add it to the reaction flask, heat to 140°C, add 8.0g (0.064mol) of 2-amino-4-hydroxy-6-methylpyrimidine and stir to dissolve, after completely dissolved, move to 28°C Rapidly cool down to 28°C in a water bath environment, then quickly add 11.9g (0.077mol) isocyanoethyl methacrylate, and maintain 28°C for addition reaction for 5 hours. During the reaction, the reaction system is always maintained at 28°C, which can inhibit It polymerizes violently, producing by-products. After the addition reaction was completed, it was vacuum filtered and washed three times with excess acetone, and the resulting white solid was dried in vacuo to obtain 17.58 g of methacrylic acid 2-[[[(1,6-dihydro-4-methyl-6 -Oxo-2-pyrimidinyl)amino]carbonyl]amino]ethyl ester, yield 98.00%, purity 99.5%.

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Abstract

The invention discloses a synthesis method of a pyrimidine aminoethyl methacrylate compound, and relates to the technical field of lithium batteries. The synthesis method is characterized in that an aminopyrimidine compound and isocyano ethyl methacrylate are subjected to an addition reaction to obtain the pyrimidine aminoethyl methacrylate compound. According to the method, by-products generated by a violent polymerization phenomenon after isocyano ethyl methacrylate is added can be effectively inhibited, and the yield of the product is further improved; and according to the synthesis method, the yield reaches 97.89% or above, and the purity reaches 99.5% or above.

Description

technical field [0001] The invention relates to the technical field of lithium batteries, in particular to a synthesis method of pyrimidineaminoethyl methacrylate compounds. Background technique [0002] Lithium-ion batteries are currently widely used in the new energy vehicle market. There are many problems in the manufacturing process of lithium-ion batteries. The core problem is the life of the battery electrolyte. Lithium ions mainly rely on lithium ions between the positive and negative electrodes. Mobile to work, by adding organic electrolyte additives can significantly improve battery life, which contains methacrylic acid 2-[[[(1,6-dihydro-4-methyl-6-oxo-2-pyrimidinyl)amino ] Carbonyl] amino] ethyl ester electrolyte additive can significantly improve the stability of the battery electrolyte. [0003] And its synthetic method of 2-[[[(1,6-dihydro-4-methyl-6-oxo-2-pyrimidinyl) amino] carbonyl] amino] ethyl methacrylate on the market is relatively complicated, As a res...

Claims

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Application Information

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IPC IPC(8): C07D239/47H01M10/0567
CPCC07D239/47H01M10/0567Y02E60/10
Inventor 刘鹏田丽霞张茜张民彭鹏鹏郝俊侯荣雪王军葛建民武利斌闫彩桥许晓丹闫朋飞杨世雄赵光华高山林胜赛李庆占邢艳召
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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