2,2'-Butylidenebis(6-tert-butyl-p-cresol) synthesis

Yield:4081-14-5 91.7%

Reaction Conditions:

with sulfuric acid;sodium dodecyl-sulfate in water at 90; for 10 h;Inert atmosphere;Temperature;

Steps:

1

In a 250 mL three-necked flask equipped with a reflux condenser, a thermometer and an electric stirrer, under nitrogen protection,32.8 g of 4-methyl-6-tert-butylphenol and 72 g of a sulfuric acid aqueous solution having a mass fraction of 10%Sodium dodecyl benzene sulfonate 0.3g, stirring evenly,Slowly drippingN-butyraldehyde 9g,After the reaction was carried out at a temperature of 90 ° C for 10 hours, 45 g of the recovered ethyl acetate was added,Stirring even after the separation, the lower sulfuric acid aqueous solution can be added in high concentrations of sulfuric acid, so that the mass fraction of 5%, transported back to the original process recycling; the upper ethyl acetate solution cooled to 0 after the filter, the filtrate distilled Ethyl acetate, sent to the original process for the next production, filter cake into a vacuum oven drying (vacuum 0.06MPa, time 5 hours), dried product 35.1g, yield the product of 91.7%, purity 99.90

References:

CN106146258,2016,A Location in patent:Paragraph 0029; 0030