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ChemicalBook CAS DataBase List Antioxidant 565
991-84-4

Antioxidant 565 synthesis

3synthesis methods
By taking 2,6-di-tert-butylphenol as the raw material, and then adding sodium nitrite solution dropwise to form an intermediate product of 2,6-di-tert-butyl-4-nitrosophenol solution, with the added Rayon Nickel is used as a catalyst and carbon monoxide is used instead of hydrogen as a reducing agent to overcome hydrogen as a reducing agent. The pressure in the hydrogenation process is high, which is prone to explosion problems. At the same time, iron crystals are added to remove excess carbon monoxide and avoid the effects of carbon monoxide toxicity. The impurities are removed by filtration, and other by-products will not be formed, which can greatly increase the yield of antioxidant 565, and the product purity is high.
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Yield:991-84-4 42.0 g

Reaction Conditions:

in toluene at 60; for 5 h;Time;

Steps:

3.4 4. Preparation of 565 4-[(4,6-dioctylthio-1,3,5-triazin-2-yl)amino]-2,6-di-tert-butylphenol

To the reaction solution of the compound II, 120 ml of toluene (the toluene layer after solvent removal in the preparation of the compound III) was added at 25 ° C,The compound III produced in the step 2 is added dropwise, after the addition is completed,After heating to 60 ° C and reacting for 5 hours, the final product was produced, and the content of the sample was 98.21%. The final product was allowed to stand for stratification, and the organic layer was taken out, washed twice with water, and desolvated under reduced pressure.Crystallization was carried out by adding 250 ml of methanol, and the mixture was filtered and dried to give 42.0 g.

References:

CN109651280,2019,A Location in patent:Paragraph 0046; 0053; 0054; 0055; 0062; 0063; 0064; 0071

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