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A technology for triazinone and compound, applied in the field of preparation of triazinone, can solve the problems of high treatment cost, difficult to treat waste water, high pollution, etc., and achieve the effects of simple preparation method, reduced raw material cost, high yield and content
Active Publication Date: 2020-11-10
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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Abstract
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Problems solved by technology
However, a large amount of high-salt, high-pollution and difficult-to-treat wastewater is produced in the production process of triazinone, and the treatment cost is high.
Method used
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Embodiment 1
[0032] 50 grams of chloropinacolone (0.37mol) were dissolved in 50 milliliters of water, then 17 grams of sodium hydroxide was added, heated to 110 degrees Celsius, and reacted for 2 hours. When GC detection showed that there was no raw material, stop heating and cooling. Poured into water, extracted with ethyl acetate, the organic layer was washed with water and 5% sodium chloride solution successively, dried, and spin-dried to obtain 40.5 g of a light yellow liquid (Compound I), with a yield of 89% and a purity of 96%.
Embodiment 2
[0034] 50 grams of chloropinacolone (0.37mol) were dissolved in 50 milliliters of water, followed by adding 61 grams of potassium carbonate, heated to 120 degrees Celsius, and reacted for 2 hours. When GC detection showed that there was no raw material, the heating and cooling was stopped. Poured into water, extracted with ethyl acetate, the organic layer was washed with water and 5% sodium chloride solution successively, dried, and spin-dried to obtain 34 g of light yellow liquid (Compound I), with a yield of 73% and a purity of 92%.
Embodiment 3
[0038] Suspend 30 grams of Compound I (0.26mol) in water, add 10 grams of 10% Pt / C, feed air at a rate of 1 g / min, keep the temperature at 25 degrees Celsius, and add 79.5 grams of sodium carbonate (0.75mol) in batches , keep the pH value at 8-9, react for 5 hours to obtain the aqueous solution of compound II (wherein the mass concentration of compound II is 20%), adjust the aqueous solution of compound II to pH value=2~3 with 30% concentrated hydrochloric acid, then heat up To 50 degrees centigrade, then add 28 grams of thiocarbamide (0.26mol), after adding, dropwise add 30% concentrated hydrochloric acid to adjust the pH value=2, heat up to 80 degrees centigrade and react for 5 hours, filter, and dry to obtain 50 grams of triazone, Yield 95%, purity 99%.
[0039] The impact of catalyst application times on triazone yield is shown in the following table:
[0040] 10% Pt / C application times Triazinone weight Yield purity 1 51 97 99 5 50 95 99 ...
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Abstract
The invention relates to a triazinone preparation method, which comprises: carrying out a hydrolysis reaction on 1-chloropinacolone at a temperature of 80-140 DEG C under the actions of a solvent andan alkali to obtain a compound I, wherein the solvent is water; carrying out an oxidation reaction on the compound I in the presence of oxygen by using Pt as a catalyst under a neutral or weakly basiccondition to obtain a compound II; and carrying out a ring closure reaction on the compound II and thiocarbohydrazide under the catalysis of an acid to obtain triazinone, wherein the structure formula of the compound I is defined in the specification, and the structure formula of the compound II is defined in the specification. According to the present invention, 1-chloropinacolone is used as theraw material, and the water is used as the solvent, such that the generation of high salt wastewater can be avoided; Pt is used as the catalyst, and oxygen is used as the oxidant, such that the use of hydrogen peroxide can be avoided, and the catalyst can be recycled so as to reduce the raw material cost; and the production method is simple, meets the environmentally friendly requirement, and issuitable for industrial production, and the yield and the content of the final product are high.
Description
technical field [0001] The invention specifically relates to a preparation method of triazone. Background technique [0002] Metribuzin, English common name: metribuzin, is a systemic selective herbicide, mainly absorbed through roots, stems and leaves can also be absorbed. It has a good control effect on annual broad-leaved weeds and some grass weeds, and is one of the main herbicide varieties in my country. Among them, triazinone is an essential raw material for the synthesis of azimidone, and its production process mainly includes four main processes: chlorination, alkali hydrolysis, oxidation and cyclization. [0003] The authorized notification number is CN105218472B, which discloses a preparation method of triazone, which reacts dichloropinazone at 80-140°C for 1-3 hours in the presence of an organic solvent and a catalyst, and then undergoes post-treatment to obtain the compound Ⅰ. Compound I is oxidized at 0-40°C for 1-4 hours in the presence of an oxidizing agent ...
Claims
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