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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: 2008-07-16
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
Comparison scheme
Effect test

Embodiment 1

[0009] Add 400kg of water, 850kg of dichloromethane (10kmol), 177kg of hydroxylamine hydrochloride (2.5kmol), and 1kg of catalyst crown ether in the reaction kettle, start stirring, dropwise add 316kg of chloropivaloyl chloride (2kmol), and control the temperature below 10- 30°C, dropwise time is 2 hours, then add sodium hydroxide dropwise, control the pH value between 6-10, dropwise time is about 4 hours, continue to stir for 1 hour after adding, stop stirring, let stand for 1 hour, Layering, after two extractions, dichloromethane was evaporated to obtain 4,4-dimethylisoxazol-3-one, and its average yield reached more than 95%, and its content was more than 90%.

Embodiment 2

[0011] A kind of synthetic method of 4,4-dimethylisoxazol-3-ketone, get hydroxylamine hydrochloride 70kg (1kmol), make catalyst with crown ether, take the mixed liquid of methylene chloride 284kg (3.33kmol) and water 300kg as Solvent, control the reaction temperature at 0-30°C, add chloropivaloyl chloride dropwise for 2 hours, add 158kg (1kmol) dropwise in total, then add sodium hydroxide dropwise for 2 hours, keep the pH of the solution at 6-10, and then stir for 1 hour After standing still for separation, extract with dichloromethane, and desolventize to obtain the product; the catalyst dosage is 0.2% of the weight of chloropivaloyl chloride.

Embodiment 3

[0013] 4, the synthetic method of 4-dimethylisoxazol-3-ketone, get hydroxylamine hydrochloride 1.4kmol, make catalyst with polyethylene glycol-600, take the mixed liquid of methylene chloride 850kg (10kmol) and water 300kg as solvent , control the reaction temperature at 0-30°C, add chloropivaloyl chloride dropwise for 3 hours, add 158kg (1kmol) dropwise in total, then add sodium hydroxide dropwise for 5 hours, keep the pH of the solution = 6-10, and stir for another 3 hours Stand to separate layers, extract the water layer with dichloromethane, and desolventize to obtain the product; the catalyst dosage 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 synthesis method of 4,4-dimethylisoxazol-3-one. Background technique [0002] Clomazone is a herbicide widely used in soybean fields, which can control most broadleaf weeds and some grass weeds, and can be used both before and after emergence; 4,4-dimethylisoxazol-3-one is The intermediate of the agricultural herbicide clomazone, the current data report that in the synthesis of the intermediate 4,4-dimethylisoxazol-3-one, water is mainly used as a solvent, and then reacted with o-chlorobenzyl chloride to obtain isochlorobenzyl In the process of bacazone, when the intermediate 4,4-dimethylisoxazol-3-one is produced, hydroxylamine hydrochloride is taken, water is used as a solvent, the reaction temperature is controlled at 0-30°C, and chloropivaloyl chloride and Sodium Hydroxide, Reaction Equation [0003] [0004] Extraction is carried...

Claims

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Application Information

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