A kind of synthetic method of environment-friendly 2,3,5-trimethylhydroquinone
A technology of trimethylhydroquinone and a synthesis method, applied in 2 fields, can solve problems such as high synthesis cost, difficult separation and preparation, and achieve the effects of low cost, low corrosiveness and stable reaction
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Embodiment 1
[0042] Add 900mL of formic acid to a 3L three-necked flask equipped with a condenser tube, a calcium chloride drying tube, a constant pressure dropping funnel and a thermometer, and slowly add 1,2,4-trimethylbenzene (120g, 1moL, 1.0Eqv ), slowly raise the temperature to 50°C, as the temperature of the reaction system rises, the system gradually dissolves, after the system dissolves, slowly add 30% hydrogen peroxide (906 grams, 8moL, 8Eqv ), as the reaction occurs, the system continues to heat up, The final system temperature was kept at about 90°C for 5 hours. After the reaction was detected by TLC, the reaction system was lowered to room temperature, the system was transferred to a 10L extractor, 1600mL of toluene (800mL×2) was added to extract the product, the extracts were combined, and transferred to Add 1740 grams of 30% saturated aqueous solution of sodium dithionite to a 5L three-necked flask, and continue mechanical stirring to raise the temperature of the reaction syst...
Embodiment 2
[0044]Add 900mL of formic acid to a 3L three-necked flask equipped with a condenser tube, a calcium chloride drying tube, a constant pressure dropping funnel and a thermometer, and slowly add 1,2,4-trimethylbenzene (120g, 1moL, 1.0Eqv ), slowly raise the temperature to 50°C, as the temperature of the reaction system rises, the system gradually dissolves, after the system dissolves, slowly add 30% hydrogen peroxide (906 grams, 8moL, 8Eqv ), as the reaction occurs, the system continues to heat up, The final system temperature was kept at about 80°C for 5 hours. After the reaction was detected by TLC, the reaction system was lowered to room temperature, the system was transferred to a 10L extractor, 1600mL of toluene (800mL×2) was added to extract the product, the extracts were combined, and transferred to Add 1740 grams of 30% saturated aqueous solution of sodium dithionite to a 5L three-necked flask, and continue mechanical stirring to raise the temperature of the reaction syste...
Embodiment 3
[0046] Add 900mL of formic acid to a 3L three-necked flask equipped with a condenser tube, a calcium chloride drying tube, a constant pressure dropping funnel and a thermometer, and slowly add 1,2,4-trimethylbenzene (120g, 1moL, 1.0Eqv ), slowly raise the temperature to 50°C, as the temperature of the reaction system rises, the system gradually dissolves, after the system dissolves, slowly add 30% hydrogen peroxide (906 grams, 8moL, 8Eqv ), as the reaction occurs, the system continues to heat up, The final system temperature was kept at about 100°C for 5 hours. After the reaction was detected by TLC, the reaction system was lowered to room temperature, and the system was transferred to a 10L extractor, and 1600mL of toluene (800mL×2) was added to extract the product. The extracts were combined and transferred to Add 1740 grams of 30% saturated aqueous solution of sodium dithionite to a 5L three-necked flask, and continue mechanical stirring to raise the temperature of the react...
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