Process for preparing diphenyl sulphone formyl paraquinone dioxime
A technology for dibenzoyl-p-quinone dioxime and p-benzoquinone dioxime, which is applied in the field of catalytic synthesis of dibenzoyl-p-quinone dioxime, can solve the problems of serious pollution, high treatment cost, non-compliance with greening and the like, and achieves the The effect of high utilization of raw materials
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Embodiment 1
[0012] In the first step, put 2.0g of p-benzoquinone dioxime into the reactor, add 50ml of chloroform, stir evenly, and raise the temperature to 55°C, stir at constant temperature for 30min; then add 4.3g of benzoyl chloride dropwise to the reaction system within 10min In, reaction 4h.
[0013] In the second step, the reaction system is cooled to room temperature, then quickly filtered with suction, the filtrate is recovered into the reactor, the filtered solid is washed three times with 15ml of chloroform, and then recrystallized with chloroform to obtain the product dibenzoyl-p-quinonedioxime , all the chloroform consumed in this process is recycled to the reactor. The yield (calculated as p-benzoquinonedioxime) was 73.2%.
[0014] The recovery experiment was performed on the recovered solvent according to the above ratio, and the yield was 74.1%.
Embodiment 2
[0016] In the first step, put 2.0g of p-benzoquinone dioxime into the reactor, add 50ml of chloroform, stir evenly, and raise the temperature to 55°C, stir at constant temperature for 30min; then add 4.7g of benzoyl chloride dropwise to the reaction system within 10min In, reaction 4h.
[0017] In the second step, the reaction system is cooled to room temperature, then quickly filtered with suction, the filtrate is recovered into the reactor, the filtered solid is washed three times with 15ml of chloroform, and then recrystallized with chloroform to obtain the product dibenzoyl-p-quinonedioxime , all the chloroform consumed in this process is recycled to the reactor. The yield (calculated as p-benzoquinone dioxime) was 85.7%.
[0018] The recovery experiment was performed on the recovered solvent according to the above ratio, and the yield was 88.1%.
Embodiment 3
[0020] In the first step, put 2.0g of p-benzoquinone dioxime in the reactor, add 50ml of chloroform, stir evenly, and raise the temperature to 55°C, stir at constant temperature for 30min; then add 5.5g of benzoyl chloride dropwise to the reaction system within 10min In, react 3h.
[0021] In the second step, the reaction system is cooled to room temperature, then quickly filtered with suction, the filtrate is recovered into the reactor, the filtered solid is washed three times with 15ml of chloroform, and then recrystallized with chloroform to obtain the product dibenzoyl-p-quinonedioxime , all the chloroform consumed in this process is recycled to the reactor. The yield (calculated as p-benzoquinonedioxime) was 70.2%.
[0022] The recovery experiment was performed on the recovered solvent according to the above ratio, and the yield was 72.2%.
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