Antioxidant 1010 synthesis

Yield:6683-19-8 98%

Reaction Conditions:

with sodium montmorillonite in methanol at 130 - 140; under 22502.3 - 30003 Torr; for 7 h;Inert atmosphere;Reagent/catalyst;

Steps:

1 Example 1

The 584gβ- (3,5- di-t-butyl-4-hydroxyphenyl) propionate,68 g of pentaerythritol,0.58 g of sodium montmorillonite,50 ml of methanol was added to the flask with mechanical stirring,Thermometer socket,In a 1000 ml four-necked flask equipped with a stirrer,Heating the material with a heating jacket,And stirring is started,The temperature reaches 130-140 ,Filled with nitrogen,The reaction system pressure was controlled at 3-4 MPa,7h after the end of the reaction,Cooling to 25 ,filter,drying,Pentaerythritol tetrakis [β - (3,5-di-tert-butyl-4-hydroxyphenyl) propionate]. The results of liquid chromatography, the results shown in Figure 1,The absorption peak at the retention time of 2.643 min belongs to 3.5 methyl ester with the content of 0.43%.The absorption peak at the retention time of 3.29 min is attributed toPentaerythritol tris [β- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate], content of 0.69%;The absorption peak at 3.84 min was assigned to dealkylationPentaerythritol tetrakis [β- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate] in 0.55%;The absorption peak at the retention time of 4.747 min is attributed toPentaerythritol tetrakis [β- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate] in 96.45%Therefore, the synthesis of pentaerythritol tetrakis [[beta] - (3,5-di-tert-butyl-4-hydroxyphenyl) propionate] in the present method meets the industry standard of not less than 94%. The yield of the product was 98%.

References:

CN106278894,2017,A Location in patent:Paragraph 0017; 0018; 0019