Antioxidant 1035 synthesis

Yield:41484-35-9 99.3%

Reaction Conditions:

with alumina-supported potassium hydroxide at 120 - 160; for 0.5 h;Catalytic behavior;Inert atmosphere;Temperature;

Steps:

1-7
Add 58.98g (0.202mol) 3-(3,5-di-tert-butyl-4-hydroxyphenyl) methyl propionate into a four-necked flask equipped with a stirrer, condenser, thermometer and nitrogen inlet.1.18g (2% of the mass of methyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate) KOH/Al2O3 catalyst,Replace the air in the reaction system with nitrogen,Heat the system to 120°C,Add 12.2g (0.1mol) of thiodiglycol in four times,The time interval for each addition of thiodiglycol is 30 min. At the end of feeding, the temperature is raised to 160,Keep the temperature at 160±5 for 30min.Turn on the vacuum pump to raise the vacuum in the flask (vacuum -0.09MPa),Incubate the reaction for 2 hours to remove the by-product methanol produced by the reaction. After the reaction, the temperature was raised to 170°C,After maintaining 170±5 and reducing pressure for 30min,Open the nitrogen valve and purge for 10 minutes, alternately until there is no methyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate coming out,After the reaction, the vacuum was broken with nitrogen, cooled to 70°C, and filtered to obtain a colorless or slightly yellow transparent product 1, with a yield of 99.3%.The purity is 99.2%.

References:

Xinxiang Rui Feng New Materials Co., Ltd.;Wang Qianqian;Xu Kun;Fan Jinfeng CN111484432, 2020, A Location in patent:Paragraph 0059-0079

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