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A kind of crystallization purification process of pyraclostrobin condensation intermediate

A technology of pyraclostrobin and intermediates, which is applied in the crystallization and purification process field of pyraclostrobin condensation intermediates, can solve the problems of unfavorable purification and refining of final products, great influence on the purity of final products of condensation intermediates, etc., and achieve Good crystallization effect, high crystallization yield and simple equipment

Active Publication Date: 2018-07-03
张掖市大弓农化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In actual production, it is found that the purity of the condensation intermediate has a great influence on the purity of the subsequent reaction product and the final product. Generally, the purity of the condensation intermediate is within a certain range, and every 1% decrease in the purity will make the subsequent reduction product The purity of pyraclostrobin decreased by about 1.5%, the purity of the esterification product decreased by about 2%, and the purity of the final product pyraclostrobin decreased by about 3.5%, which is very unfavorable for the purification of the final product

Method used

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Embodiment 1

[0013] A kind of crystallization purification process of pyraclostrobin condensation intermediate:

[0014] In parts by weight, 80 parts of pyraclostrobin condensation intermediates with a purity of 94.3% were added to the crystallization tank, and then 400 parts of anhydrous methanol and 20 parts of N,N-dimethylformamide were pumped in, Start stirring, heat up to 60-80°C, reflux for 30-60min, cool down to 35-45°C, then slowly add 3 parts of triethylamine dropwise to the crystallization kettle, after the dropwise addition, keep the temperature at 35-45°C, Continue to stir for 15-30min, lower the temperature slowly, control the cooling rate at 5-10°C / h, lower the temperature to 3-8°C, keep stirring for 1-2 hours, filter with suction, collect the mother liquor into the mother liquor tank, and use 3- Rinse twice with a small amount of anhydrous methanol at 8°C, take out the filter cake, and dry it in an oven to obtain high-purity pyraclostrobin condensation intermediate crystals....

Embodiment 2

[0017] A kind of crystallization purification process of pyraclostrobin condensation intermediate:

[0018] In parts by weight, 80 parts of pyraclostrobin condensation intermediates with a purity of 93.6% were added to the crystallization tank, and then 600 parts of anhydrous methanol and 20 parts of N,N-dimethylformamide were pumped in, Start stirring, heat up to 60-80°C, reflux for 30-60min, cool down to 35-45°C, then slowly add 3 parts of triethylamine dropwise to the crystallization kettle, after the dropwise addition, keep the temperature at 35-45°C, Continue to stir for 15-30min, lower the temperature slowly, control the cooling rate at 5-10°C / h, lower the temperature to 3-8°C, keep stirring for 1-2 hours, filter with suction, collect the mother liquor into the mother liquor tank, and use 3- Rinse twice with a small amount of anhydrous methanol at 8°C, take out the filter cake, and dry it in an oven to obtain high-purity pyraclostrobin condensation intermediate crystals....

Embodiment 3

[0021] A kind of crystallization purification process of pyraclostrobin condensation intermediate:

[0022] In parts by weight, 80 parts of pyraclostrobin condensation intermediates with a purity of 91.8% were added to the crystallization tank, and then 800 parts of anhydrous methanol and 25 parts of N, N-dimethylformamide were pumped in. Start stirring, heat up to 60-80°C, reflux for 30-60min, cool down to 35-45°C, then slowly add 5 parts of triethylamine dropwise to the crystallization kettle, after the dropwise addition, keep the temperature at 35-45°C, Continue to stir for 15-30min, lower the temperature slowly, control the cooling rate at 5-10°C / h, lower the temperature to 3-8°C, keep stirring for 1-2 hours, filter with suction, collect the mother liquor into the mother liquor tank, and use 3- Rinse twice with a small amount of anhydrous methanol at 8°C, take out the filter cake, and dry it in an oven to obtain high-purity pyraclostrobin condensation intermediate crystals...

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Abstract

The invention discloses a crystallizing and purifying process of pyraclostrobin condensation intermediates .The technology includes the steps that 80-100 parts of pyraclostrobin condensation intermediates, 400-1000 parts of absolute methanol and 20-25 parts of N,N-dimethylformamide are added into a crystallizing kettle by weight, the temperature is raised to be 60-80 DEG C, back flowing is conducted for 30-60 minutes, the temperature is lowered to be 35-45 DEG C, 3-5 parts of triethylamine is dropwise added, the temperature is kept to be 35-45 DEG C, stirring is continued for 15-30 minutes, the temperature is cooled to be 3-8 DEG C, temperature keeping and stirring are conducted for 1-2 hours, suction filtration is conducted, a mother solution is collected into a mother solution tank, a filter cake is drip washed twice with a small amount of absolute methanol at 3-8 DEG C, the filter cake is taken out to be dried in an oven, and then high-purity pyraclostrobin condensation intermediate crystal substances are obtained .The crystallizing and purifying process is good in crystallizing effect, crystallizing products are high in purity, the crystallizing yield is high, applied devices are simple, and the process is suitable for industrial production and can produce remarkable economic benefits .

Description

technical field [0001] The invention belongs to the technical field of pesticide production, and relates to a process for crystallization and purification of pyraclostrobin condensation intermediates. Background technique [0002] Pyraclostrobin, also known as pyraclostrobin, English common name: Pyraclostrobin, chemical name: N-[2-[[1-(4-chlorophenyl)pyrazol-3-yl]oxymethyl]benzene Base]-Methyl N-methoxycarbamate. Pyraclostrobin belongs to the methoxyacrylate fungicides, which mainly acts on the mitochondria of fungi, preventing electron transfer and thus inhibiting fungal growth. Pyraclostrobin can prevent and control all types of fungal pathogens with a wide bactericidal spectrum. It is mainly used to prevent and control grape powdery mildew and downy mildew; wheat powdery mildew and rust; barley leaf rust; banana black leaf streak disease; tomato early and late disease and other diseases. Pyraclostrobin is effective against various diseases of various crops including w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D231/22
CPCC07D231/22
Inventor 胡华金张向东常科文胡灵玲李俊
Owner 张掖市大弓农化有限公司
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