Compound for preventing Chinese tussah silk-worm disease caused by tachina flies and use method
A technology of compound and carbon atom, which is applied in the field of tussah moth control, can solve the problems of unacceptable control effect in production, sericulture production application has not been reported, and has not been patented, etc., and achieves a novel insecticidal mechanism , high efficiency and high killing activity
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Embodiment 1
[0019] Synthesis of compound XA01: Add 0.03mol of fipronil and 40mL of THF into a three-necked flask with a condenser and magnetic stirring, add NaH (0.036mol) in batches under ice-water bath conditions, stir for 0.5h, and then drop Dissolve 0.03 mol of butyryl chloride in 10 mL of THF, raise the temperature to 85 ° C and reflux overnight, stop the reaction, remove the solvent by rotary evaporation, add Na 2 CO 3 Solution, adjust the pH to 7.0-8.0 to remove acidic impurities. Adopt ethyl acetate to extract 3 times, combine organic phase, filter after anhydrous magnesium sulfate drying, adsorb on activated silica gel, adopt dry packing column, through column chromatography (V (petroleum ether): V (ethyl acetate) = 4:1) 4.92g product was obtained, the yield was 32.3%. Determination of compound melting point, using Bruker AvanceⅢ400 1 H NMR test confirmed its structure (XA01, see Table 2).
Embodiment 2
[0021] Synthesis of compound XA13: using similar steps as in Example 1, the difference is: during the reaction, the raw material butyryl chloride was replaced with trichloroacetyl chloride, and the column chromatography mixed solvent V (petroleum ether): V (ethyl acetate ) adjusted to 3:1. 7.01 g of product (XA13, see Table 2 for structure) can be prepared with a yield of 40.1%.
[0022] According to the similar method of Example 1 and 2, all the compounds in Table 2 can be prepared; the difference is: during the reaction, the raw material butyryl chloride is replaced with isobutyryl chloride, hexanoyl chloride, heptanoyl chloride, octanoyl chloride, crotonyl chloride, methacryloyl chloride, Cinnamoyl chloride, furoyl chloride, monochloroacetyl chloride, dichloroacetyl chloride, 2-chloropropionyl chloride, 3-chloropropionyl chloride, and phenylacetyl chloride can be used to prepare products XA02-12, 14-16. Among them, compounds WX-1 and WX-2 are compounds disclosed in the lit...
Embodiment 3
[0028] Taking XA01 as an example to prepare the emulsifiable concentrate dispersant of the compound
[0029] According to the calculated ratio, 10.10g of compound XA01 (purity calculated at 99%) was dissolved in 84.90g of solvent ethylene glycol methyl ether, then 5.00g of agricultural emulsifier was added to remove B3, and stirred at high speed for 0.5h to make XA01 with a mass concentration of 5.00 % homogeneous emulsifiable concentrate, dilute with water to the desired concentration when used.
[0030] The rest of the compounds were prepared into emulsifiable concentrates of the compounds using the same process as above.
[0031] 3. Biological Activity Evaluation
[0032] Test method: In a silkworm farm in Fengcheng City, Liaoning Province, the oak trees in the silkworm farm are mainly 2 to 3-year-old Mongolian oak and oak. Take the tussah variety Da Sanyuan as the test insect, use 500 3-6-day-old fifth-instar tussah silkworms per treatment, disperse them in 6-10 twig oak...
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