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Preparation method of 3, 3-dimethyl-2-oxobutyric acid and triazinone

A technology of oxobutyric acid and dimethyl, applied in the field of pesticides, can solve problems such as being unfavorable to industrialized production, unable to be effectively recycled and reused, avoid high-salt wastewater and solid waste, reduce raw material costs, and achieve high yields. Effect

Inactive Publication Date: 2021-06-22
NUTRICHEM LAB CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The same method produces high-salt wastewater containing heavy metals, and uses more catalysts, which cannot be effectively recycled and reused, which is not conducive to industrial production

Method used

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  • Preparation method of 3, 3-dimethyl-2-oxobutyric acid and triazinone

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preparation example Construction

[0023] According to the first aspect of the present invention, there is provided a method for preparing 3,3-dimethyl-2-oxobutanoic acid, the method comprising: in the presence of a catalyst, at a pH of 7-13, containing oxygen The body is an oxidizing agent, and the step of oxidizing 3,3-dimethyl-2-hydroxybutyric acid and / or its salt.

[0024] According to the present invention, preferably, the oxygen-containing gas is oxygen and / or air. In view of improving reaction efficiency, the oxygen-containing gas is preferably oxygen. Considering cost reduction, the oxygen-containing gas is preferably air.

[0025] According to the present invention, preferably, the catalyst is one or more of ruthenium dioxide, Pt-C, Pd-C and ruthenium trichloride; more preferably, the catalyst is ruthenium dioxide, Pt One or more of -C and Pd-C. From the viewpoint of further improving the yield, ruthenium dioxide is more preferable.

[0026] Preferably, the catalyst is used in an amount of 3,3-dime...

Embodiment 1

[0056] 1) In a 500ml four-necked bottle, put 192g (0.32mol) of 20% by weight NaOH into it, heat up to 50°C under stirring, add 16.8g (0.1mol) of molten dichloropinatone dropwise at 50-70°C, drop After completion of the heat preservation reaction for 1 hour, GC analysis showed that the reaction was complete, the reaction solution was lowered to room temperature, adjusted to pH 2-3 with aqueous hydrochloric acid (concentration: 10% by weight), extracted with ethyl acetate, and the organic phase was removed to obtain 3,3- Dimethyl-2-hydroxybutyric acid (GC-MS M + =132) solid with a purity of 98% by weight and a yield of 95%.

[0057] 2) Put 13.5g of 3,3-dimethyl-2-hydroxybutyric acid into a 100ml autoclave, add 30% by weight of sodium hydroxide aqueous solution to completely dissolve, adjust the pH to 12, and add ruthenium dioxide (1mol%) 0.13g, stir and raise the temperature to 110°C, feed oxygen, keep the pressure at 4MPa, react for 8h, and GC analyzes that the reaction of raw...

Embodiment 2

[0059] 1) In a 500ml four-necked bottle, put 192g (0.32mol) of 20% by weight NaOH into it, heat up to 50°C under stirring, add 16.8g (0.1mol) of molten dichloropinatone dropwise at 50-70°C, drop After completion of the heat preservation reaction for 1 hour, GC analysis showed that the reaction was complete, the reaction solution was lowered to room temperature, adjusted to pH 2-3 with aqueous hydrochloric acid (concentration: 10% by weight), extracted with ethyl acetate, and the organic phase was removed to obtain 3,3- Dimethyl-2-hydroxybutyric acid solid, purity 98% by weight, yield 95%.

[0060] 2) Put 13.5g of 3,3-dimethyl-2-hydroxybutyric acid into a 100ml high-pressure reactor, add saturated potassium bicarbonate aqueous solution to completely dissolve, adjust the pH to 8, and add the catalyst ruthenium dioxide recovered in Example 1 , stirred and raised the temperature to 60°C, fed oxygen, kept the pressure at 6MPa, reacted for 8h, and the raw materials controlled in the...

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Abstract

The invention relates to the field of pesticides, and discloses a preparation method of 3, 3-dimethyl-2-oxobutyric acid and triazinone. The preparation method of the 3, 3-dimethyl-2-oxobutyric acid provided by the invention comprises the step of oxidizing the 3, 3-dimethyl-2-oxobutyric acid and / or a salt thereof by taking oxygen-containing gas as an oxidizing agent in the presence of a catalyst under the condition that the pH value is 7-13. According to the method disclosed by the invention, the 3, 3-dimethyl-2-hydroxybutyric acid and / or the salt thereof is taken as the raw material, and oxygen or air is used for replacing other oxidants, so that high-salinity wastewater and solid waste are avoided, the cost of the raw material is reduced, and the method is simple to operate and suitable for industrial production.

Description

technical field [0001] The invention relates to the field of pesticides, in particular to a preparation method of 3,3-dimethyl-2-oxobutanoic acid and triazone. Background technique [0002] Mecitrione (CAS: 21087-64-9) is a systemic selective herbicide, mainly absorbed through roots, stems and leaves. For annual broad-leaved weeds and some gramineous weeds such as soybean, potato, tomato, alfalfa, asparagus, sugarcane and other crop fields, control Polygonum, amaranth, quinoa, mustard greens, bitter weed, chickweed, buckwheat vine, fenugreek, and Artemisia annua , ghost needle grass, foxtail grass, commelina, cocklebur, nightshade, crabgrass, wild oats, etc. have good control effects. Low toxicity to humans and animals, low toxicity to fish, aquatic organisms, birds and bees. No abnormality was found in the chronic toxicity test. [0003] 3,3-Dimethyl-2-oxobutanoic acid (or trimethylpyruvate) is an important intermediate for the preparation of mecitrione, and its structur...

Claims

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Application Information

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IPC IPC(8): C07C51/373C07C59/185C07D253/075
CPCC07C51/373C07D253/075
Inventor 张晟吴国林王晓磊李衍强王磊乔振
Owner NUTRICHEM LAB CO LTD
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