Synthetic method of 3-chlorine-2-hydrazinopyridine

Abstract

The invention discloses a synthetic method of 3-chlorine-2-hydrazinopyridine. The synthetic method is characterized by comprising the following steps: uniformly mixing 2-fluorine-3-chloropyridine and hydrazine hydrate, adding an alcohol solvent, reacting for 3-5 hours at a room temperature, drying the solvent, and carrying out rotary evaporation, thus obtaining the 3-chlorine-2-hydrazinopyridine. The synthetic method of the 3-chlorine-2-hydrazinopyridine has the advantages that the operation process is simple, the high-yield high-quality product can be obtained without heating flux, the product yield can reach 99.53%, and the product purity can reach 99.95%.

Description

technical field [0001] The invention relates to a synthesis method of 3-chloro-2-hydrazinopyridine, which belongs to the field of fine chemical industry. Background technique [0002] 3-Chloro-2-hydrazinopyridine is an important intermediate for the synthesis of new ryanodine receptor insecticides, chlorantraniliprole and cyantraniliprole. These insecticides mainly act on insect calcium ion channels, and anesthetize the muscle relaxation of insects. Regarding the preparation of 3-chloro-2-hydrazinopyridine, currently a large amount of hydrazine hydrate is mainly used to react with 2,3-dichloropyridine. For example, in the foreign patent WO2008 / 134969 A1, dioxane is used as a solvent, and the reflux reaction is carried out for 20 2,3-dichloropyridine was obtained in 1 hour, and the product yield was 71%; Chinese patent CN101550130A directly refluxed 2,3-dichloropyridine and hydrazine hydrate for 4 hours, and the yield was 68.5%; in the above method, 3-chloro-2 The yields of...

AI Technical Summary

Problems solved by technology

Regarding the preparation of 3-chloro-2-hydrazinopyridine, currently a large amount of hydrazine hydrate is mainly used to react with 2,3-dichloropyridine. For example, in the foreign patent WO2008 / 134969 A1, dioxane is used as a solvent, and the reflux reaction is carried out for 20 2,3-dichloropyridine was obtained in 1 hour, and the product yield was 71%; Chinese patent CN101550130A directly refluxed 2,3-dichloropyridine and hydrazine hydrate for 4 hours, and the yield was 68.5%; in the above method, 3-chloro-2 The yield of hydrazinopyridine is relatively low, waste of materials, high cost and difficult to effectively implement in industrial production

And in Chinese patent CN102249991 A, with 2,3-dichloropyridine and hydrazine hydrate as raw materials, add polar solvent (methanol, ethanol, dimethylformamide, dimethylacetamide, tetrahydrofuran), reflux reaction 4-8 After hours, drop to room temperature suction filtration and promptly obtain 3-chloro-2 hydrazinopyridine, the yield of this kind of method product can reach 95%-99%, but the raw material of this kind of method is 2,3-dichloropyridine, chlorine The leaving property is not high, and it needs to be heated and refluxed for a long time before it can be removed, which is not ideal in terms of economy