Yield:15520-11-3 126 g

Reaction Conditions:

with 1,2-ethanediol, dibenzoate;dihydrogen peroxide;magnesium sulfate;sodium hydroxide in water;Petroleum ether at 40; pH=10; for 2.5 h;Reagent/catalyst;Temperature;

Steps:

6; 7 Example 6

The reactor was successively charged with 273 g deionized water, 300 g of a 0.2 wt% Methocel K99 solution, 1.5 g of a 3.4 wt% MgS0₄ solution, and 45.3 g 50% NaOH solution. Next, 15.4 g 70% H2O2 was added, while maintaining the temperature at 40°C. Under intensive stirring, a mixture of 125.2 g 4-t- butylcyclohexyl chloroformate, 15.5 g ethyleneglycol dibenzoate, and 8.5 g petroleum ether 60-80 was dosed within 1 minute at 40°C. After 60 minutes, the pH dropped to 10.0 and was then maintained at this value during 90 minutes, while dosing NaOH-50%. The mixture was neutralized with HCI-18% to pH 7 and filtered over a G-3 glass filter and washed with deionized water. The solids were dried in air yielding 126 g of a powdery formulation of di(4-tert- butylcyclohexyl) peroxydicarbonate in EGDB with a peroxide assay of 84.7%.

References:

WO2019/121366,2019,A1 Location in patent:Page/Page column 12; 13