Antioxidant3114 synthesis

Yield:27676-62-6 92.3%

Reaction Conditions:

with hexamethylenetetramine in methanol;water at 120 - 140; under 4500.45 Torr; for 6 h;Autoclave;Inert atmosphere;Pressure;

Steps:

1-2 Example 2
To a 1L autoclave with mechanical stirring, thermometer socket, pressure gauge, nitrogen replacement port, 178g of 2,6-di-tert-butylphenol, 24.48g of paraformaldehyde, 41.28g of isocyanuric acid and 4.4g of urotropine were added. 4.4g, under vacuum, nitrogen replacement for more than 3 times, after the last nitrogen replacement, under the condition of negative pressure (-0.01Mpa), 1000mL aqueous solution of 70% by volume of methanol is pumped into the reactor, and then Nitrogen gas was introduced into the apparatus to a pressure of 0.6 MPa, and the temperature was raised under a nitrogen atmosphere. After the temperature was raised to 120 ° C for 2 hours, the temperature was further raised to 140 ° C for 4 hours, and the reaction was completed. The circulating water of the reaction kettle was cooled to 58 ° C to obtain a crude product, and the crude product was directly filtered, and the solid matter was dissolved in a 70% by volume aqueous solution of methanol at a concentration of 70 ° C, and recrystallized by cooling, and then anhydrous at 55 ° C. The methanol was washed twice or more and dried to obtain a white crystalline material, which was the target product hindered phenolic antioxidant 3114, and the yield was 92.3%.

References:

Yingkou Fengguang New Materials Co., Ltd.;Wang Lei CN108707122, 2018, A Location in patent:Paragraph 0020; 0021; 0028; 0029

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