Co-crystals of boscalid and triazoles
A technology of boscalid and co-crystallization, applied in the field of controlling fungi, can solve the problems of expensive crystallization inhibitors and surfactants, unfavorable environment, etc.
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example 1
[0108] Example 1: Preparation of co-crystals of boscalid and tebuconazole according to the invention by anti-solvent crystallization and precipitation:
[0109] 300.0 g of boscalid and 270.0 g of tebuconazole were charged into a glass kettle. To this mixture was added 2992 g of dichloroethane. The slurry was heated to 40-45°C for 10 to 12 hours. The solvent was evaporated under reduced pressure at 40-45°C. Hexane (400.0 g) was added to the reduced mass and the mixture was stirred at 30-35°C for 30 minutes to precipitate the product. The precipitated product was filtered and dried to obtain 566 g of white solid. The melting point of the solid, recorded by differential scanning calorimetry, showed an endothermic peak at 90.01 °C.
[0110] The compound was analyzed by HPLC to determine the molar ratio of boscalid and tebuconazole in the cocrystal ( Figure 5 ).
[0111] Wherein the molar ratio of boscalid: tebuconazole is 50.58:48.92.
example 2
[0112] Example 2: Preparation of co-crystals of boscalid and hexaconazole according to the invention by anti-solvent crystallization and precipitation:
[0113] 20.0 g of boscalid and 18.0 g of hexaconazole were charged into a glass kettle. To this mixture was added 200 g of dichloroethane. The slurry was heated to 40-45°C for 10 to 12 hours. The solvent was evaporated under reduced pressure at 40-45°C. Hexane (100.0 g) was added to the reduced mass and the mixture was stirred at 30-35°C for 30 minutes to precipitate the product. The precipitated product was filtered and dried to obtain 37.2 g of white solid. The solid melting point recorded by differential scanning calorimetry showed an endothermic peak at 103.4 °C.
example 3
[0114] Example 3: Preparation of co-crystals of boscalid and cybaconazole according to the invention by anti-solvent crystallization and precipitation:
[0115] 20.0 g of boscalid and 17.0 g of cyproconazole were charged into a glass kettle. To this mixture was added 200.0 g of dichloroethane. The slurry was heated to 40-45°C for 10 to 12 hours. The solvent was evaporated under reduced pressure at 40-45°C. Hexane (100.0 g) was added to the reduced mass and the mixture was stirred at 30-35°C for 30 minutes to precipitate the product. The precipitated product was filtered and dried to obtain 36.1 g of white solid. The solid melting point recorded by differential scanning calorimetry showed an endothermic peak at 99.03 °C.
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