TERT-AMYLPEROXY 2-ETHYLHEXYL CARBONATE synthesis

Yield:-

Reaction Conditions:

with pyridine;sodium hydroxide at 35; for 3 h;Temperature;

Steps:

1.3; 1.4; 2.3; 2.4; 3.3; 3.4; 4.3; 4.4
(3) Add a metered amount of 30% sodium hydroxide drops and a pyridine catalyst to the upper tert-amyl hydrogen peroxide, and then add a metered amount of 2-ethylhexyl chloroformate to make the tert-amyl hydrogen peroxide: The molar ratio of 2-ethylhexyl chloroformate: base=1.5:1:1.8, and the amount of pyridine is 4.5% of tert-amyl hydroperoxide. Stirring is continued, the reaction temperature is controlled to 35°C, the reaction time is 3 hours, and the reaction time is 3 hours. The reaction time is 3 hours, and the mixture is allowed to stand still, lower to room temperature, and separate carefully. The upper organic layer is the target product tert-amyl peroxide-2-ethylhexyl carbonate.(4) Add 30% sodium hydroxide to the upper product, the weight is 10% of the product, continue to stir, stand still, and separate the liquid. The upper organic layer is the product tert-amyl peroxide-2-ethylhexyl carbonate. Then add a metered 5% potassium sulfide to the product, the weight is 6% of the product. Adjust the pH to 10 with sulfuric acid, keep stirring for 1 hour at 30°C, stand still, separate the liquid, the upper organic layer is the product tert-amyl peroxide-2-ethylhexyl carbonate, and then add the product at 200Kg/h to In the thin film evaporator, the temperature is 50°C and the vacuum degree is controlled at -0.98MPa. The tert-amyl peroxide-2-ethylhexyl carbonate is discharged from the discharge port under the thin film evaporator, and the content is measured and weighed. The content is 99.31%.

References:

CN112300045, 2021, A Location in patent:Paragraph 0029; 0032-0033; 0034; 0037-0038; 0039; 0042-0043