Preparation method of buprofezin drug molecules with escherichia coli inhibition effect
The technology of a drug molecule and Escherichia coli is applied in the field of preparation of thiazide drug molecules, which can solve the problem of low yield and achieve the effects of high product yield, good antibacterial effect and simple operation.
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Embodiment 1
[0021]
[0022] Add 17g of 3-carbonyl-4-(4-methylphenyl)butyronitrile and 3.5g of aluminum trichloride into a mixture of 17g of methanol and 170g of ether in a high-pressure reactor, stir for 10min, and at 0°C, Pass hydrogen chloride gas into the reaction kettle to make the pressure in the reaction kettle reach 0.05MPa, keep the pressure constant, slowly rise to room temperature, stir and react for 15h, filter the reaction solution, add 100mL of n-hexane to the reaction solution under the protection of argon, If there is solid precipitation, the filter cake is quickly added to 150mL of methanol after rapid suction filtration under the protection of argon, and then put into the high-pressure reactor again, and the air in the reactor is vacuum-extracted, and then 85g of liquid ammonia is passed into the reactor. Irrigation reaction method, raise the temperature, make the reaction kettle reach 0.2MPa, stir and react for 20h, distill off the solvent, treat the concentrate with e...
Embodiment 2
[0024] Add 17g of 3-carbonyl-4-(4-methylphenyl)butyronitrile and 3.5g of cobalt trichloride into a mixed solution of 17g of methanol and 170g of diethyl ether in a high-pressure reactor, stir for 10min, and at 0°C, Pass hydrogen chloride gas into the reaction kettle to make the pressure in the reaction kettle reach 0.05MPa, keep the pressure constant, slowly rise to room temperature, stir and react for 9h, filter the reaction solution, add 100mL of n-hexane to the reaction solution under the protection of argon , there is solid precipitation, and the filter cake is quickly added to 150mL of methanol after rapid suction filtration under the protection of argon, and then put into the high-pressure reactor again, the air in the reactor is vacuum-extracted, and then 85g of liquid ammonia is passed into the reactor, and the liter High temperature, make the reaction kettle reach 0.2MPa, stir and react for 20h, evaporate the solvent, treat the concentrate with ether and filter to obta...
Embodiment 3
[0026]Add 17g of 3-carbonyl-4-(4-methylphenyl)butyronitrile and 3.5g of cobalt trichloride into a mixed solution of 17g of methanol and 170g of diethyl ether in a high-pressure reactor, stir for 10min, and at 0°C, Pass hydrogen chloride gas into the reaction kettle to make the pressure in the reaction kettle reach 0.05MPa, keep the pressure constant, slowly rise to room temperature, stir and react for 9h, filter the reaction solution, add 100mL of n-hexane to the reaction solution under the protection of argon , there is solid precipitation, and the filter cake is quickly added to 150mL of methanol after rapid suction filtration under the protection of argon, and then put into the high-pressure reactor again, and the air in the reactor is vacuum-extracted, and then 51g of liquid ammonia is passed into the reactor, and the liter High temperature, make the reaction kettle reach 0.2MPa, stir the reaction at room temperature for 20h, evaporate the solvent, treat the concentrate wit...
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