SYP-9080 crystal and preparation method thereof
A technology for tetrachloraniliprole and crystals, which is applied in the field of tetrachlorantraniliprole crystals and their preparation, and can solve the problems that the product cannot be separated from the system and the like
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1 4
[0072] The preparation of embodiment 1 tetrachlorantraniliprole crystal
[0073]Take 144g of ethyl acetate, add 20g of 2-amino-3,5-dichloro-N-methylbenzamide, and slowly drop 3-bromo-1-(3,5- Dichloropyridin-2-yl)-1H-pyrazole-5-carbonyl chloride 35g, dropwise added for 2 hours, after the dropwise addition, the temperature was raised to 80°C for reaction, after 5 hours of reaction, stop heating, in the cycle assembled in the system The condensing device is fed with circulating water to cool down to 52°C at a cooling rate of 0.1°C / min, and continues to pass through circulating cooling water at 25.2°C, and cools down to 30°C within 2 hours, and finally passes through circulating frozen brine at -15.2°C, 2.5 Cool down to 0°C within hours. Use a G3 filter funnel to filter for about 1 minute to obtain crystals, and dry at 40°C for 4 hours to obtain crystals of tetraclotraniliprole.
Embodiment 2 4
[0074] The preparation of embodiment 2 tetrachlorantraniliprole crystals
[0075] Take 120g of tetrahydrofuran, add 25g of 2-amino-3,5-dichloro-N-methylbenzamide, and slowly add 3-bromo-1-(3,5-dichloro Pyridin-2-yl)-1H-pyrazole-5-formyl chloride 40g, added dropwise for 3 hours, raised the temperature to 65°C and reacted for 8 hours after the dropwise addition, passed circulating water into the circulating condensing device equipped with the system at a rate of 0.30 Cool down to 45°C at a cooling rate of °C / min, continue to pass in 20°C circulating cooling water, cool down to 25°C within 0.5 hours, and finally pass through -18°C circulating frozen brine, and cool down to -5°C within 0.5 hours. Use a G3 filter funnel to filter the obtained crystals in about 1 minute and dry them at 30°C for 5 hours to obtain crystals of tetraclotraniliprole.
Embodiment 3 4
[0076] The preparation of embodiment 3 tetrachlorantraniliprole crystals
[0077] Take 160g of acetonitrile, add 30g of 2-amino-3,5-dichloro-N-methylbenzamide, and slowly add 3-bromo-1-(3,5-dichloro Pyridin-2-yl)-1H-pyrazole-5-carbonyl chloride 40g, add dropwise for 0.5 hours, raise the temperature to 90°C for 1 hour after the dropwise addition, and cool down to 65°C naturally after the reflux, keep the temperature for 1 hour, in the system The assembled circulating condensing device is fed with circulating water to cool down to 55°C at a cooling rate of 0.03°C / min, continue to pass through 30°C circulating cooling water, cool down to 35°C within 3 hours, and finally pass through -5°C circulation Freeze the brine and cool down to 5°C within 4 hours. Use a G3 filter funnel, filter for about 1 minute to complete the filtration, and dry the obtained crystals at 50° C. for 3 hours to obtain crystals of tetraclotraniliprole.
PUM
| Property | Measurement | Unit |
|---|---|---|
| particle diameter | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More