Antioxidant3114 synthesis
- Product Name:Antioxidant3114
- CAS Number:27676-62-6
- Molecular formula:C48H69N3O6
- Molecular Weight:784.08
50-00-0
108-80-5
128-39-2
27676-62-6
To a 1L autoclave equipped with a mechanical stirrer, a thermometer socket, a manometer and a nitrogen displacement port, 178 g of 2,6-di-tert-butylphenol, 24.48 g of paraformaldehyde, 41.28 g of isocyanuric acid, and 4.4 g of urotropine were added sequentially. The system was vacuumed and nitrogen replacement was repeated more than three times, and after the last nitrogen replacement, 1000 mL of 70% v/v methanol aqueous solution was pumped into the reactor under -0.01 MPa negative pressure. Subsequently, the system was charged with nitrogen to a pressure of 0.6 MPa. Under the nitrogen atmosphere, the temperature was gradually increased to 120°C and maintained for 2 hours, and then continued to increase to 140°C and maintained for 4 hours to complete the reaction. At the end of the reaction, the reactor was cooled to 58°C by circulating water to obtain the crude product. After the crude product was filtered, the solid was dissolved in 70% by volume methanol aqueous solution, cooled and recrystallized. The recrystallized product was washed at least twice with anhydrous methanol at 55 °C and dried to give the white crystalline target product, hindered phenolic antioxidant 3114, in 92.3% yield.
50-00-0
892 suppliers
$10.00/25g
108-80-5
514 suppliers
$6.00/25g
128-39-2
363 suppliers
$5.00/25g
27676-62-6
239 suppliers
$9.00/25g
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