Isoxazoline compound with optical activity and application thereof
An isoxazoline and compound technology, applied in the field of isoxazoline compounds, can solve the problems of no optical isomers, no involving the same or different optical isomers, no involving optical isomers, etc.
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Embodiment 1
[0097] The preparation of embodiment 1 compound 3
[0098]
[0099] 1) Preparation of ethyl (S)-3-(5-amino-2-chloro-4-fluorophenyl)-5-methyl-4,5-dihydro-5-isoxazolecarboxylate
[0100] Put 25g of Amylose tris (3,5-dimethylphenylcarbamate) silica gel into the chromatographic column, which will contain 1g of 3-(5-amino-2-chloro-4-fluorophenyl)-5-methyl-4,5-dihydro The 5ml dichloromethane solution of ethyl 5-isoxazolecarboxylate (prepared with reference to the method in CN105753853) is adsorbed in the chromatographic column, and is separated by Biotage rapid preparation chromatography, and the corresponding components are collected to obtain optical isomerism (R)-3 -(5-Amino-2-chloro-4-fluorophenyl)-5-methyl-4,5-dihydro-5-isoxazolecarboxylic acid ethyl ester 0.47g (optical purity 99.8%, melting point 105-106 ℃), (S)-3-(5-amino-2-chloro-4-fluorophenyl)-5-methyl-4,5-dihydro-5-isoxazolecarboxylic acid ethyl ester 0.46g (optical Purity 99.4%, melting point 104-105°C).
[0101] ...
Embodiment 2
[0107] Embodiment 2 Indoor herbicidal activity assay
[0108] The herbicidal activity testing method of compound of the present invention is as follows:
[0109] Quantitative gramineous weeds (barnyardgrass, golden foxtail) and broad-leaved weeds (zinnia, velvetleum) seeds were respectively sown in paper cups with a diameter of 7 cm filled with nutrient soil, and covered with soil 1 cm after sowing, pressed, After watering, they were cultivated in the greenhouse according to conventional methods. Gramineae weeds grow to 2-3 leaf stage, and broad-leaved weeds 2-4 leaf stage stem and leaf spray treatment; pre-emergence soil spray treatment is carried out 24 hours after sowing. According to the test design dose, carry out the spray treatment (spray pressure 1.95kg / cm2) on the crawler crop sprayer (Engineer Research Ltd. design and production, UK). 2 , spray volume 500L / hm 2 , crawler speed 1.48km / h). The experiment was repeated 3 times. After treatment, the test materials ar...
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