Efficient synthesis method of antioxidant 168
A synthesis method and antioxidant technology are applied in the field of efficient synthesis of antioxidant 168, which can solve the problems of high product purification requirements, low product purity, and insufficient effect, and achieve high product yield, high purity, good effect
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Embodiment 1
[0019] ①. Add 252.15g 2,4-di-tert-butylphenol, 5.7g 4-dimethylaminopyridine and 8.5g triethylamine into a 500ml three-necked flask, then mix 387g xylene and 55.35g phosphorus trichloride solution was added slowly, the temperature was raised to 50°C, and the reaction was carried out for 5 hours;
[0020] 2. The reaction solution obtained in step 1. was heated up to 160° C., reacted for 1.5 h, and hydrogen chloride and xylene were distilled out under reduced pressure;
[0021] ③. Cool the reaction solution after vacuum distillation in step ② to 90°C, add isopropanol, stir for 1 hour, then cool to room temperature, filter with suction and dry to obtain 255.2g of antioxidant 168, yield 98.6% (using trioxide Phosphorus is used as the basis to calculate the yield), the melting point is 184.5~185.3°C, and the purity is 99.7%.
Embodiment 2
[0023] ①. Add 252.15g of 2,4-di-tert-butylphenol, 8.8g of 4-dimethylaminopyridine and 8.8g of triethylamine into a 500ml three-necked flask, then mix 276g of xylene and 55.35g of phosphorus trichloride solution was added slowly, heated to 60°C, and reacted for 2 hours;
[0024] 2. The reaction solution obtained in step 1. is warmed up to 130° C., reacted for 5 hours, and distilled out hydrogen chloride and xylene under reduced pressure;
[0025] ③. Cool the reaction solution after vacuum distillation in step ② to 90°C, add isopropanol, stir for 1 hour, then cool to room temperature, filter with suction and dry to obtain 254.9g of antioxidant 168, yield 98.5% (by trioxide The yield is calculated based on phosphorus), the melting point is 184.3~185.2°C, and the purity is 99.8%.
Embodiment 3
[0027] ①. Add 252.15g 2,4-di-tert-butylphenol, 8.5g 4-dimethylaminopyridine and 5.7g triethylamine into a 500 ml three-necked flask, then add 332g xylene and 55.35g phosphorus trichloride The mixture was added slowly, heated to 55°C, and reacted for 3.5 hours;
[0028] ②. The reaction solution obtained in step ① was heated up to 145° C., reacted for 3.5 hours, and distilled hydrogen chloride and xylene under reduced pressure;
[0029] ③. Cool the reaction solution after vacuum distillation in step ② to 90° C., add isopropanol, stir for 1 hour, cool to room temperature, filter and dry to obtain 253.4 g of antioxidant 168, yield 97.9% (by trioxide The yield is calculated based on phosphorus), the melting point is 184.1~185.4°C, and the purity is 99.7%.
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