Hapten of organophosphorus triazophos pesticide and preparation method thereof
A triazophos-like and organophosphorus-like technology, applied in the field of hapten and its preparation of organophosphorus triazophos-like pesticides, can solve the problems of organophosphorus pesticide residues, environmental pollution, threats to human health and ecological environment, etc.
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[0044] According to one aspect of the present invention, the present invention relates to a method for preparing a hapten of organophosphorus triazophos pesticides, comprising the following steps:
[0045] A method for preparing a hapten of an organophosphorus triazophos pesticide, comprising the following steps:
[0046] (a) using 1-phenyl-3-hydroxyl-1,2,4-triazole as a raw material to obtain 1-p-nitrobenzene-3-hydroxyl-1,2,4-triazole through nitration reaction;
[0047] (b) Substituting the 1-p-nitrobenzene-3-hydroxyl-1,2,4-triazole obtained in step (a) and diethylphosphoryl thiochloride to obtain diethyl (1-p-nitrogen phenyl-3-hydroxy-1,2,4-triazole) phosphorothioate;
[0048](c) Diethyl (1-p-nitrobenzene-3-hydroxyl-1,2,4-triazole) phosphorothioate obtained in step (b) is subjected to a nitro reduction reaction to obtain diethyl (1 - p-aminobenzene-3-hydroxy-1,2,4-triazole) phosphorothioate;
[0049] (d) Diethyl (1-p-aminobenzene-3-hydroxyl-1,2,4-triazole) phosphorothioa...
Embodiment 1
[0088] A preparation method of organophosphorus triazophos pesticide hapten, comprising the following steps:
[0089] (a) Add 6.0g of 1-phenyl-3-hydroxy-1,2,4-triazole into 50mL of concentrated sulfuric acid, add 2.6g of fuming nitric acid dropwise to the reaction solution at 0°C, and the addition is complete Finally, at 0°C, the reaction solution was stirred for 5 hours; figure 1 LCMS detection showed that the raw materials were consumed completely, and a product peak was generated; the 1-p-nitrobenzene-3-hydroxyl-1,2,4-triazole reaction solution was poured into ice water, and the precipitated solid was filtered first, and then dissolved in ethyl acetate After ester beating, filter to obtain light yellow solid 1-p-nitrobenzene-3-hydroxyl-1,2,4-triazole compound; 1-p-nitrobenzene-3-hydroxyl-1,2,4-triazole compound is 5.0g, the yield is 65%;
[0090] (b) 5.0g 1-p-nitrobenzene-3-hydroxyl-1,2,4-triazole, 3.7g triethylamine (Et 3 N), 0.3g 4-dimethylaminopyridine (DMAP) and 6.0g...
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