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A crude product post-treatment process for the preparation of 2-amino-4,6-dimethoxypyrimidine

A technology of dimethoxypyrimidine and amino, which is applied in the field of post-treatment process of crude products prepared from 2-amino-4,6-dimethoxypyrimidine, which can solve the problems of operation cost, increase of volatile organic compounds, volatilization and penetration Leakage and other problems, to reduce the steps of solvent recovery, reduce production costs, eliminate the effect of environmental protection pressure

Active Publication Date: 2019-08-30
HUBEI HUIDA HIGH TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The dispersant has a certain solubility to the product, resulting in product loss. At the same time, it needs to be recycled and applied, resulting in operating costs
② There are potential safety hazards
Due to the large amount of toluene dispersant, it will volatilize and leak during use (such as product filtration, dispersant recovery and mother liquor treatment, etc.), increasing the impact of volatile organic compounds (VOC, volatile organic compounds) on the factory Environmental pollution affects the health of workers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: 2-amino-4,6-dimethoxypyrimidine was distilled under reduced pressure to crystallization and granulation (purification)

[0018] 600kg of liquid crude 2-amino-4,6-dimethoxypyrimidine was transferred to a 3000L stainless steel still by vacuum for distillation under reduced pressure. After distillation, add 1200kg of pure water and 3.0kg of triethylamine to the product obtained after distillation and cooling, and heat to 80-85°C until 2-amino-4,6-dimethoxypyrimidine is completely melted, while stirring Slowly lower the temperature to 35-40°C, filter, and dry the filter cake to obtain 589.8kg of pure white crystal 2-amino-4,6-dimethoxypyrimidine, with a content of 99.95% and a single-step recovery of 98.3%.

Embodiment 2

[0019] Example 2: 2-amino-4,6-dimethoxypyrimidine was distilled under reduced pressure to crystallization and granulation (purification)

[0020] Transfer 600kg of 2-amino-4,6-dimethoxypyrimidine liquid crude product to a 3000L stainless steel still by vacuum, and carry out vacuum distillation. After the distillation, add 1800kg of pure water to the product obtained after distillation cooling and 4.0kg of ammonium carbonate, heated to 80-85°C until the 2-amino-4,6-dimethoxypyrimidine was completely melted, slowly cooled to 45-50°C while stirring, filtered, and the filter cake was dried to obtain pure 594.0 kg of white crystal 2-amino-4,6-dimethoxypyrimidine, content 99.93%, single-step recovery rate 99.0%.

Embodiment 3

[0021] Example 3: 2-amino-4,6-dimethoxypyrimidine was distilled under reduced pressure to crystallization and granulation (purification)

[0022] Transfer 600kg of 2-amino-4,6-dimethoxypyrimidine liquid crude product to a 3000L stainless steel distillation kettle by vacuum, and carry out vacuum distillation. After the distillation, add 1500kg of pure water to the product obtained after distillation cooling and 3.0kg of triethylamine, heated to 90-95°C until the 2-amino-4,6-dimethoxypyrimidine is completely melted, slowly cooled to 35-40°C while stirring, filtered, and the filter cake was dried to obtain 591.6 kg of pure white crystal 2-amino-4,6-dimethoxypyrimidine, content 99.90%, single-step recovery rate 98.6%.

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PUM

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Abstract

The invention discloses a crude product aftertreatment new technique for preparing 2-amino-4, 6-dimethoxy pyrimidine, wherein the technique includes steps of transferring a liquid crude product of 2-amino-4, 6-dimethoxy pyrimidine in a distilling kettle by vacuum, and performing depressurization and distilling; adding pure water and stabilizer to the product acquired by distilling and cooling; heating to 75-95 DEG C and melting; then stirring while slowly cooling to 30-50 DEG C; filtering the product; drying a filter cake and acquiring a white crystal particle shaped pure product of 2-amino-4, 6-dimethoxy pyrimidine. The new technique applies easy-acquired water at lower price as the dispersing agent to replace methylbenzene, xylene and other organic solvents, reduces the solvent recycling step, and further reduces the production cost. The new technique eliminates the safety hidden trouble of low-boiling and flammable organic solvent and the environment protection pressure of volatile component which can pollute the production environment; the weak alkali type stabilizer is introduced, thus the process of generating polarity impurities from dropped methyl of 2-amino-4, 6-dimethoxy pyrimidine is effectively inhibited, thus the product quality is further promoted.

Description

technical field [0001] The invention relates to a new post-treatment process of crude product of 2-amino-4,6-dimethoxypyrimidine (ADMP), an important intermediate of medicine and pesticide. Background technique [0002] 2-Amino-4,6-dimethoxypyrimidine (ADMP) is a class of excellent pyrimidine compounds, which are widely used as various pesticide intermediates. At present, among the mainstream preparation methods of ADMP, the process route using malononitrile as raw material has been focused on, and there have been many documents on process optimization. Among them, the patent CN201510575548.3, which was applied for and published by our company in 2015, proposed an optimization Scheme: The solvent-free method is adopted in the step of aromatization and cyclization reaction, the obtained crude product is distilled in high vacuum, and then an organic solvent is introduced as a dispersant for crystallization and granulation to obtain a pure product. [0003] This solution is lo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/52
Inventor 李永芳凌云王中奎
Owner HUBEI HUIDA HIGH TECH CO LTD
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