Antioxidant 168 synthesis
- Product Name:Antioxidant 168
- CAS Number:31570-04-4
- Molecular formula:C42H63O3P
- Molecular Weight:646.94
96-76-4
31570-04-4
(1) First, 11.0 g of 2,4-di-tert-butylphenol was added to a 250 mL three-neck flask. Subsequently, 22 mg of diatomaceous earth-loaded pyridine catalyst and 400 mL of a solvent mixture of methanol and toluene (1:1 by volume) were added. A magnetic stirrer, reflux condenser tube were installed and a thermometer and a dropping funnel were fixed at the remaining two ports of the three-necked flask, respectively. (2) Place the reaction apparatus in step (1) in an oil bath and programmatically warm the reaction mixture at a rate of 5 °C/10 min to 40 °C and stir the reaction mixture at this temperature. (3) A solution of 5.57 g of phosphorus trichloride dissolved in 30 mL of toluene was slowly added dropwise through a dropping funnel to the reaction system in step (2), with a controlled dropping time of 15 min. After the dropwise addition was completed, the reaction was continued to be heated to 95 °C and maintained for 30 min. Upon completion of the reaction, the solvent was removed by distillation under reduced pressure. The crude product was recrystallized with hexane to give tris(2,4-di-tert-butylphenyl) phosphite in 98.3% yield and 98.9% purity.
96-76-4
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31570-04-4
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$6.00/25g
Yield:31570-04-4 98.3%
Reaction Conditions:
Stage #1: 2,4-di-tert-Butylphenolwith pyridine in methanol;toluene at 5 - 40;
Stage #2: with phosphorus trichloride in methanol;toluene at 95; for 0.5 h;Reagent/catalyst;Temperature;
Steps:
9 Example 9 Method for synthesizing tris(2,4-di-tert-butylphenyl) phosphite
(1)First, 11.0 g of 2,4-di-tert-butylphenol was added to a three-necked flask.a diatomaceous earth-supported pyridine catalyst of 22 mg and a mixed solution of methanol and toluene in 400 mL, and then added to the rotor, and a reflux condenser,The thermometer and the dropping funnel were fixed on a three-necked flask;(2)The three-necked flask containing the reactant in the step (1) was heated under an oil bath condition at a rate of 5 degrees Celsius per ten minutes.Raise the temperature to 40 ° C,Reacting solution;(3)To the reaction liquid of the step (2), 5.57 g of phosphorus trichloride dissolved in 30 mL of toluene was added dropwise to control the dropping rate.After 15 minutes of dropwise addition, continue to heat up to 95 ° C,The reaction was kept for 30 minutes, and the solvent was distilled off under reduced pressure.Recrystallization from n-hexane,That is, the product is obtained.The yield of the final product was 98.3%.The purity was 98.9%.
References:
CN108467406,2018,A Location in patent:Paragraph 0038-0040; 0044-0046; 0050-0052; 0056-0058; 0062