Antioxidant 168 synthesis

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