Method for synthesizing chlorantraniliprole
A technology for chlorantraniliprole and benzamide, which is applied in the field of chlorantraniliprole synthesis, can solve the problems of high difficulty in industrialization, high requirements for synthesis steps, single method for synthesizing chlorantraniliprole, and the like, and achieves post-processing Simple, easy-to-use effects
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Embodiment 1
[0025] S1. Stir the solvent containing 2-amino-3-methylbenzoic acid, wherein the solvent is an ether compound, and dropwise add methylamine solution during the stirring reaction process, heat to reflux, then extract and dry to obtain N- Methyl-3-methyl-2-amino-benzamide;
[0026] S2. Dissolve N-methyl-3-methyl-2-amino-benzamide in lye, wherein the lye is an aqueous solution of potassium tert-butoxide, keep stirring for 5 minutes, and add dropwise hydrogen peroxide with a mass concentration of 30%. , temperature controlled at 12°C, after the reaction, carry out halogenation reaction with NCS to obtain N-methyl-3-methyl-2-amino-5-chloro-benzamide;
[0027] S3, select 3-aminocrotononitrile to stir, add hydrazine hydrate to mix during stirring, carry out ring closing reaction, rise to room temperature naturally and react for 3 hours, get 3-amino-5-methylpyrazole, to 3-amino Adjust the pH value to 2 during the stirring process of crotononitrile and hydrazine hydrate, and stir in i...
Embodiment 2
[0033] S1. Stir the solvent containing 2-amino-3-methylbenzoic acid, wherein the solvent is an ether compound, and dropwise add methylamine solution during the stirring reaction process, heat to reflux, then extract and dry to obtain N- Methyl-3-methyl-2-amino-benzamide;
[0034] S2, dissolving N-methyl-3-methyl-2-amino-benzamide in lye, wherein the lye is an aqueous solution of potassium tert-butoxide, stirring continuously for 10 minutes, and adding hydrogen peroxide with a mass concentration of 30% dropwise , temperature controlled at 28°C, after the reaction, carry out halogenation reaction with NCS to obtain N-methyl-3-methyl-2-amino-5-chloro-benzamide;
[0035] S3, select 3-aminocrotononitrile to stir, add hydrazine hydrate to mix during stirring, carry out ring closing reaction, rise to room temperature naturally and react for 4 hours, get 3-amino-5-methylpyrazole, to 3-amino During the stirring process of crotononitrile and hydrazine hydrate, adjust the pH value to 3,...
Embodiment 3
[0041] S1. Stir the solvent containing 2-amino-3-methylbenzoic acid, wherein the solvent is an ether compound, and dropwise add methylamine solution during the stirring reaction process, heat to reflux, then extract and dry to obtain N- Methyl-3-methyl-2-amino-benzamide;
[0042] S2. Dissolve N-methyl-3-methyl-2-amino-benzamide in lye, wherein the lye is an aqueous solution of potassium tert-butoxide, keep stirring for 8 minutes, and add dropwise hydrogen peroxide with a mass concentration of 30%. , temperature controlled at 25°C, after the reaction, carry out halogenation reaction with NCS to obtain N-methyl-3-methyl-2-amino-5-chloro-benzamide;
[0043]S3, select 3-aminocrotononitrile to stir, add hydrazine hydrate to mix during stirring, carry out ring closing reaction, rise to room temperature naturally and react for 4 hours, get 3-amino-5-methylpyrazole, to 3-amino During the stirring process of crotononitrile and hydrazine hydrate, adjust the pH value to 3, and stir in i...
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