Insecticidal synergistic composition
A composition and compound technology, applied in the directions of insecticides, biocides, animal repellents, etc., can solve the problems of short insecticidal control period, high cost, large dosage, etc. The effect of prolonging the control effect
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Embodiment 1
[0019] Embodiment 1: the preparation of formula (I) compound
[0020] Step 1: Preparation of 5-chloro-3-methyl-2-sulfinylaminobenzoyl chloride
[0021]
[0022] Thionyl chloride (36ml, 500mmol) was added to a suspension of 2-amino-5-chloro-3-methyl-benzoic acid (18.5g, 100mmol) in toluene (200ml), the mixture was heated to reflux, and Stir at temperature until rapid gas evolution subsides. The resulting solution was concentrated under reduced pressure to give a solid residue, which was dried under high vacuum. The crude solid product (23.7 g, 95%) was used in the next step without further purification.
[0023] 1 H-NMR (CDCl 3 ): 8.07 (d, 1H), 7.56 (d, 1H), 2.30 (s, 3H).
[0024] Step 2: Preparation of 2-amino-2-cyclopropylpropionitrile
[0025]
[0026] Cool endomethyl ketone (17.1 g, 203 mmol) and 101.9 ml of 2.12 M NH with ice bath 4 Cl in H 2 Solution of stock solution (216 mmol) in O in 30.6 ml of 25% ammonium hydroxide (216 mmol). KCN (14.1 g, 216 mmol) wa...
Embodiment 2
[0036] Embodiment 2: the preparation of formula (II) compound
[0037] Step 1: Preparation of tert-butyl 4-methoxymethylenepiperidine-1-carboxylate
[0038] Potassium tert-butoxide (21.3 g) was added in portions to a stirred solution of methoxymethyltriphenylphosphonium chloride (65.3 g) in anhydrous THF (500 mL) at 4°C under a nitrogen atmosphere. A bright orange color was noted and the reaction was held as such for 1 hour. tert-Butyl 4-oxopiperidine-1-carboxylate 1 (25 g) was added slowly without allowing the temperature to rise above 10° C., then the mixture was heated at room temperature overnight.
[0039] The reaction mixture was poured into water (150 mL), extracted three times with ethyl acetate (100 mL), the combined organics were washed with brine (300 mL), dried over anhydrous sodium sulfate and concentrated in vacuo to give a brown oil (50 g) . Flash chromatography [SiO 2 ; hexane, then ethyl acetate-hexane (10:90)] afforded 26.4 g (77%) of the desired enol eth...
Embodiment 3
[0057] Separately apply formula (I) compound, formula (II) compound and use formula (I) compound and formula (II) compound composition separately on 1 mu of cornfield, formula (I) compound, formula (II) compound are formulated into The emulsifiable concentrate, formula (I) compound and formula (II) compound composition is formulated into emulsifiable concentrate preparation according to various proportioning, is used for preventing and controlling Spodoptera littoralis, counts the cotton on every acre of land respectively in 2 days, 5 days and 8 days The mortality rate of Spodoptera moth, the specific dosage and effect are as follows, where the percentage of control effect refers to the mortality rate of Spodoptera littoralis, and the higher the mortality rate, the better the control effect:
[0058] Experimental results
[0059]
[0060]
[0061] The expected activity of the given two active ingredient compositions is calculated according to the Colby method, and compared...
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