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Method for synthesizing 4, 4-dimethyl-iso-xazole-3-one

A technology of dimethylisoxazole and a synthetic method, applied in 4 fields, can solve problems such as low yield, and achieve the effects of reducing three wastes and mild reaction conditions

Active Publication Date: 2006-05-24
JIANGSU CHANGQING AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Extraction is carried out after the reaction is completed, the yield is 88%, and the content is 85%; according to the prior art, the yield of 4,4-dimethylisoxazol-3-one is low

Method used

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  • Method for synthesizing 4, 4-dimethyl-iso-xazole-3-one

Examples

Experimental program
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Effect test

Embodiment 1

[0009] Add 400kg of water, 850kg (10kmol) of dichloromethane, 177kg (2.5kmol) of hydroxylamine hydrochloride, 1kg of catalyst crown ether into the reaction kettle, start stirring, add 316kg (2kmol) of chlorinated pivaloyl chloride dropwise, and control the temperature to be lower than 10- 30℃, the dripping time is 2 hours, then sodium hydroxide is dripped to control the pH value between 6-10, the dripping time is about 4 hours, after the addition, continue to stir for 1 hour, stop stirring, and let stand for 1 hour. Separate layers, extract twice, and distill off dichloromethane to obtain 4,4-dimethylisoxazol-3-one, with an average yield of more than 95% and a content of more than 90%.

Embodiment 2

[0011] A method for synthesizing 4,4-dimethylisoxazol-3-one, taking 70kg (1kmol) of hydroxylamine hydrochloride, using crown ether as a catalyst, and using a mixed liquid of 284kg (3.33kmol) of dichloromethane and 300kg of water as a catalyst Solvent, control the reaction temperature to 0-30℃, add chloropivaloyl chloride dropwise for 2 hours, add 158kg (1kmol) dropwise, and then add sodium hydroxide dropwise for 2 hours, keep the solution pH = 6-10, then stir for 1 hour Then stand for separation, extract with dichloromethane, and desolvate to obtain the product; the amount of catalyst is 0.2% of the weight of chloropivaloyl chloride.

Embodiment 3

[0013] Synthetic method of 4,4-dimethylisoxazole-3-one, taking 1.4 kmol of hydroxylamine hydrochloride, using polyethylene glycol-600 as a catalyst, and using a mixed liquid of 850 kg (10 kmol) of dichloromethane and 300 kg of water as a solvent Control the reaction temperature at 0-30℃, add chloropivaloyl chloride for 3 hours, add 158kg (1kmol) dropwise, and then add sodium hydroxide dropwise for 5 hours, keep the solution pH = 6-10, then stir and react for 3 hours Stand to separate the layers, extract the water layer with dichloromethane, and desolvate to obtain the product; the amount of the catalyst is 5% of the weight of chloropivaloyl chloride.

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Abstract

The invention discloses a method for synthesizing 4, 4-dimethyl isooxazole-3-ketone in the field of agricultural weedicide, taking hydroxylammonium chloride, using ether as catalyst, using dichloromethane water solution as solvent, controlling the reacting temperature at 0-30 deg.C, in turn dropping chloro tert-acyl chloride and sodium hydroxide, keeping pH value of solution 6-10, then blending and reacting, placing still and stratifying, using dichloromethane to extract, desolventizing and obtaining the product. And the product yield can reach 95%, and the product content is greater than 90%. The invention can be used in producing agricultural weedicide clomazone.

Description

Technical field [0001] The invention relates to the technical field of agricultural herbicide clomazone intermediates, in particular to a synthetic method of 4,4-dimethylisoxazol-3-one. Background technique [0002] Clomazone is a herbicide widely used in soybean fields. It can control most broad-leaved weeds and some gramineous weeds. It can be used before and after the seedlings; 4,4-dimethylisoxazol-3-one is The intermediate of the agricultural herbicide clomazone. The current data reported that in the synthesis of the intermediate 4,4-dimethylisoxazol-3-one, water is mainly used as the solvent, and then reacted with o-chlorobenzyl chloride to obtain the isoform In the process of oxazone, when the intermediate 4,4-dimethylisoxazole-3-one is produced, hydroxylamine hydrochloride is used, water is used as the solvent, the reaction temperature is controlled at 0-30℃, and chloropivaloyl chloride and Sodium hydroxide, reaction equation [0003] [0004] After the reaction is comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D261/04
Inventor 王建荣吉志扬
Owner JIANGSU CHANGQING AGROCHEMICAL CO LTD
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