Preparation method of azole acetone with high yield and low emission

A high-yield technology of oxazolam, applied in the field of preparation of pymetrozine intermediate oxazolidone, can solve the problems of high comprehensive production cost, large sewage discharge, low product purity, etc., and achieves reduction of discharge and water content. , the effect of reducing side reactions

A high-yield technology of oxazolam, applied in the field of preparation of pymetrozine intermediate oxazolidone, can solve the problems of high comprehensive production cost, large sewage discharge, low product purity, etc., and achieves reduction of discharge and water content. , the effect of reducing side reactions

CN103254150AInactive Publication Date: 2013-08-21ANHUI YANGZI CHEM
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Embodiment 1

[0018] A preparation method of azole acetone with high yield and low emission, comprising the following steps: in a 1000ml reaction bottle, a stirrer, a thermometer, a constant pressure dropping funnel and a condenser are installed, and (solvent) dichloroethane is added at room temperature 320g, (phase transfer catalyst) dodecyltrimethylammonium chloride 2g, (acid-binding agent) sodium bicarbonate 122g, oxadiazolone 150g, start stirring, heat, when the temperature rises to 50°C, start to drop Chloroacetone 128g, the dropping time is controlled at 6 hours, heat preservation reaction at 55-60°C for 1 hour, heat up to 65°C heat preservation reaction for 7 hours, the color of the solution is transparent light yellow, after sampling and analysis is qualified, cool down to 30°C Left and right, suction filtration, filter out inorganic salts, the obtained filtrate is desolventized by decompression method, vacuum precipitation control end point vacuum degree is -0.095Mpa, end point temp...

Embodiment 2

[0020] In a 1000ml reaction flask, install a stirrer, a thermometer, a constant pressure dropping funnel and a condenser, add (solvent) dichloroethane 320ml, (phase transfer catalyst) tetrabutylammonium bromide 3g, (bound Acid agent) sodium bicarbonate 115g, oxadiazolone 150g, start stirring, heat, when the temperature rises to 55°C, start to add 153g of chloroacetone dropwise, the dropping time is controlled at 5 hours, and the temperature is kept at 55-60°C for 2 hours. Raise the temperature to 60-65°C and keep it warm for 8 hours; during the process of adding chloroacetone dropwise and keeping warm and refluxing, the gaseous phase gas is condensed by the condenser and then flows into the glass water separator for water separation. A total of 30ml of light components are separated, and the sampling analysis is qualified Afterwards, cool down to about 30°C, discharge and filter with suction, and filter out inorganic salts. The obtained filtrate is desolvated by a decompression...

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Abstract

The invention relates to a preparation method of azole acetone with high yield and low emission. The preparation method comprises the following steps of: putting a solvent, oxadiazolone, a phase transfer catalyst and an acid binding agent into a reaction kettle, dripping halogen acetone at the temperature of 45 DEG C-70 DEG C, keeping the reaction dripping time to be 2-4h, adopting an azeotropic dewatering way for removing water out of a system during the reaction process, cooling a solution after dewatering to 28 DEG C-32 DEG C, emptying, performing suction filtration, performing decompression on filtrate to remove low-boiling point substances and a solvent, namely chlorinated alkane, controlling the vacuum degree at a terminal point at -0.095MPa, controlling the temperature at the terminal point of decompression distillation to be not more than 75 DEG C, and ending decompression desolvation when no condensed liquid flows down in a condenser to obtain an azole acetone product. The azeotropic dewatering way or a drying agent is adopted for dewatering in synthesis reaction, and then the water is continuously removed out of the reaction system, so that the water content in the synthesis system can be reduced as far as possible, the occurrence of side effects can be reduced, the yield can be improved, the cost is reduced, the emission of sewage is also reduced, and the preparation method is efficient and environment-friendly.

Description

technical field [0001] The present invention relates to a kind of preparation method of pesticide insecticide intermediate, more specifically, the present invention relates to a kind of preparation method of producing pymetrozine intermediate azole acetone. Background technique [0002] Pymetrozine belongs to pyridine or triazinone insecticides. It is a brand-new non-biocide insecticide. It was first developed by Ciba-Geigy in Switzerland in 1988. Pests showed excellent control effect. Studies using electropenetration graph (EPG) technology have shown that no matter in drip, feeding or injection experiments, as soon as aphids or planthoppers come into contact with pymetrozine, they will immediately produce a stylet blocking effect, stop feeding immediately, and eventually starve to death , and this process is irreversible. Pyridoxone has no knockdown activity and does not produce direct toxicity to insects. Therefore, pymetrozine has an excellent function of blocking insec...

Claims

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Application Information

Patent Timeline
21 Aug 2013
Publication
CN103254150A
IPC
C07D271/113
Inventors
黄建忠; 欧阳建峰