Cyclopropyl-containing compound, preparation and application methods thereof, and bactericide
A compound, cyclopropyl technology, applied in the field of pesticides, fungicides and fungicides, can solve problems such as prolonged use time, irrational use, and pathogen resistance, and achieve excellent control effects and good market development prospects.
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Embodiment 1
[0061] This embodiment is used to illustrate the preparation method of the compound shown in formula (1-1)
[0062]
[0063] (1) At 25°C, add 1,3-dichloroacetone (1mol) into 1L of 2M diethyl ether hydrochloride solution, then add tert-butyl nitrite (1mol), continue the reaction at 25°C for 10h, and remove Diethyl ether, after cooling, obtain the crude product of the compound shown in formula (2-1), and wash with 1-chlorobutane, filter, collect filter cake; And the filtrate is recrystallized, filter, also obtain formula (2 The compound shown in -1) was combined to obtain the pure product of the compound shown in formula (2-1) after merging two batches.
[0064] (2) At 25°C, add sodium bicarbonate (5mol) to 1L of the compound (1mol) shown in formula (2-1) in dichloromethane solution, then add 2,6-difluorostyrene (1mol) Add slowly, continue to stir and react for 4h, after the reaction is completed, filter and remove the solvent in the filtrate to obtain the compound represent...
Embodiment 2
[0068] This embodiment is used to illustrate the preparation method of the compound shown in formula (3-1)
[0069]
[0070] Ethyl bromoacetate (12mmol), cesium carbonate (20mmol) and tetrabutylammonium iodide (1mmol) were successively added to the acetonitrile solution of 3-methyl-5-trifluoromethylpyrazole (10mmol), 50°C The mixture was stirred and reacted for 6 hours. After the reaction was completed, it was filtered, the filtrate was concentrated, 20 mL of ethyl acetate was added, extracted and washed with 20 mL*3 of water, concentrated, and purified by normal phase silica gel column chromatography to obtain the compound represented by formula (3-1).
Embodiment 3
[0072] This embodiment is used to illustrate the preparation method of the compound shown in formula (4-1)
[0073]
[0074] Add the compound (10mmol) represented by formula (3-1) into anhydrous tetrahydrofuran solution, under nitrogen protection, at -78°C, slowly add 22mL of lithium bis(trimethylsilyl)amide (1.0M) tetrahydrofuran solution , reacted for 10 min, then added vinyl sulfate (12 mmol) anhydrous tetrahydrofuran, gradually raised to 25 ° C, and continued to react for 3 h. After the reaction was completed, it was quenched with saturated ammonium chloride aqueous solution, extracted with ethyl acetate, dried and concentrated, and purified by column chromatography to obtain the compound represented by formula (4-1).
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