Synthetic method of imidacloprid
A synthetic method and technology of imidacloprid, which is applied in the field of synthesis of the insecticide imidacloprid, can solve the problems of poor product purity, low product purity, long reaction cycle, etc., and achieve the promotion of positive reaction balance, high catalytic activity, and reduction of side effects. The effect of the product
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[0023] A kind of synthetic method of imidacloprid of the present invention, its synthetic steps are as follows:
[0024] ① Add amines to the reactor first, then add 2-chloro-5-chloromethylpyridine and solvent in sequence, heat and reflux for 2 hours, then cool to 45°C to obtain a catalyst solution, in which the amines and 2-chloro The molar ratio of -5-chloromethylpyridine is 0.8~1.5:1, and the mass ratio of 2-chloro-5-chloromethylpyridine to solvent is 1:5;
[0025] ②Then add solvent, 2-nitroiminoimidazolidine, and 1 / 5 amount of alkali metal hydroxide to the catalyst solution in sequence, heat to 45°C and keep for 30 minutes under stirring, the solvent and 2-nitroiminoimidazolidine The mass ratio is 5~10:1;
[0026] ③After the heat preservation is over, add 9.1%~16.7% of the solvent solution of 2-chloro-5-chloromethylpyridine dropwise to the reaction solution, add dropwise for 30min each time, 4 times in total, and add to the reaction solution after each dropwise addition A...
Embodiment 1
[0033] Embodiment 1 Concrete synthetic steps are as follows:
[0034] ①Add 0.9g 1,8-diazabicyclo[5.4.0]undec-7-ene to the reactor first, then add 1.2g 2-chloro-5-chloromethylpyridine and 6.0g methanol , after heating to reflux for 2 hours, cooled to 45°C to obtain 8.1g catalyst solution;
[0035] ②Then add 390.3g methanol, 78.06g 2-nitroiminoimidazolidine and 4g sodium hydroxide to 8.1g catalyst solution in sequence, and heat to 45°C for 30min while stirring;
[0036] ③ After the heat preservation is over, add 9.1% methanol solution of 2-chloro-5-chloromethylpyridine dropwise to the reaction solution, dropwise for 30 minutes each time, for a total of 4 times, and add 890.1g of 2-chloro-5-chloropyridine dropwise in total For the methanol solution of picoline, add 4g sodium hydroxide to the reaction solution after each dropwise addition, for a total of 4 times, and keep the reaction for 1h after the last addition of sodium hydroxide;
[0037] ④ After the heat preservation reac...
Embodiment 2
[0038] Embodiment 2 Concrete synthetic steps are as follows:
[0039] ① First add 8.75g of triethylamine to the reactor, then add 9.3g of 2-chloro-5-chloromethylpyridine and 46.7g of ethanol in sequence, heat to reflux for 2 hours, then cool to 45°C to obtain 64.8g of catalyst solution;
[0040]②Then add 1.82kg of ethanol, 182.14g of 2-nitroiminoimidazolidine, and 15.68g of potassium hydroxide to 64.8g of the catalyst solution in sequence, and heat to 45°C for 30min while stirring;
[0041] ③ After the heat preservation is over, add 16.7% ethanol solution of 2-chloro-5-chloromethylpyridine dropwise to the reaction solution, dropwise for 30 minutes each time, 4 times in total, and add 970.1g of 2-chloro-5-chloropyridine dropwise in total For the ethanol solution of picoline, add 15.68g potassium hydroxide to the reaction solution after each dropwise addition, for a total of 4 times, and keep the reaction for 2h after the last addition of potassium hydroxide;
[0042] ④ After t...
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