Method for preparing 2,3,5-trimethylhydroquinone
A technology of trimethylphenol and p-benzoquinone, applied in the field of preparation 2, which can solve the problems of troublesome separation of product and solvent, excessive catalyst, high separation cost, etc.
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Embodiment 1
[0033] In a 150 ml four-neck flask equipped with a condenser, a stirring paddle, a dropping funnel and a vent tube, add 80 grams of water, 17 grams of copper chloride dihydrate and 7 grams of anhydrous lithium chloride, and then add 0.68 grams of benzyl Triethylammonium chloride, stirred vigorously, heated to 40°C, passed oxygen through the glass tube, the flow rate was 300ml / min, began to drop 13.6g of molten 2,3,6-trimethylphenol, within 2 hours After the addition was completed, the reaction was performed for another 4 hours after the dropwise addition. After the reaction, the oil layer was directly taken for GC analysis, and the purity of 2,3,5-trimethylbenzoquinone was 93%. The oil phase was distilled under reduced pressure to obtain 13.6 g of 2,3,5-trimethylbenzoquinone with a yield of 90.0%, which was analyzed by GC again and the purity was 99.5%. MS: m / z 150 (M + )...
Embodiment 2
[0035] The 150 milliliter four-necked bottle equipped with condenser, stirring paddle, dropping funnel and ventilation tube was placed in the ultrasonic reactor, and 80 grams of water, 17 grams of copper chloride dihydrate and 7 grams of anhydrous lithium chloride were added, and then Add 0.68 g of benzyltriethylammonium chloride, stir vigorously, heat to 40°C, pass oxygen through the glass tube at a flow rate of 300 ml / min, turn on the ultrasonic wave at a frequency of 20KHz, and start to drop molten 2, Add 13.6 grams of 3,6-trimethylphenol within 2 hours, and react for another 4 hours after the dropwise addition. After the reaction, the oil layer was directly taken for GC analysis, and the purity of 2,3,5-trimethylbenzoquinone was 94%. The oil phase was distilled under reduced pressure to obtain 13.7 g of 2,3,5-trimethylbenzoquinone with a yield of 91.3%, which was analyzed by GC again and the purity was 99.6%.
Embodiment 3
[0037] The 150 milliliter four-necked bottle equipped with condenser, stirring paddle, dropping funnel and ventilation tube was placed in the ultrasonic reactor, and 80 grams of water, 17 grams of copper chloride dihydrate and 7 grams of anhydrous lithium chloride were added, and then Add 0.6 g of PEG300, stir vigorously, heat to 40°C, pass oxygen through the glass tube, the flow rate is 300 ml / min, turn on the ultrasonic wave at the same time, the ultrasonic frequency is 20KHz, start to drop the molten 2,3,6-trimethyl 13.6 grams of phenol was added within 2 hours, and then reacted for 4 hours after the dropwise addition. After the reaction, the oil layer was directly taken for GC analysis, and the purity of 2,3,5-trimethylbenzoquinone was 94%. The oil phase was distilled under reduced pressure to obtain 13.8 g of 2,3,5-trimethylbenzoquinone with a yield of 92.0%, which was analyzed by GC again and the purity was 99.7%.
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