A kind of method of synthesizing 4-bromocarbazole
A synthetic method, bromocarbazole technology, applied in the field of organic synthesis, can solve the problems of expensive raw materials, high cost, and inability to produce in large quantities, and achieve the effect of easy-to-obtain raw materials and low production costs
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example 1
[0020] 1) Add 44.1 g (0.28 mol) of o-chloronitrobenzene and 19.7 g (0.31 mol) of copper powder into a 500 mL three-necked round bottom flask equipped with a stirrer, a thermometer, and a reflux condenser. The mixture was heated to 200 °C and kept for 12 h.
[0021] Through chromatographic tracking detection, the reaction is stopped when the content of o-chloronitrobenzene in the raw material is less than 2%, cooled to room temperature, and 150 mL of dichloromethane is added to the reaction system for extraction. The reaction solution was washed with 450 mL*3 times of water, stirred to obtain a viscous solid, and then recrystallized through 200 mL of methanol. 52.6 g of light yellow solid 2,2-dinitrobiphenyl was obtained with a yield of 77%.
[0022] 2) Under the protection of an inert gas, put 48.8g (0.20mol) of light yellow 2,2-dinitrobiphenyl into a 500mL three-necked reaction flask equipped with a mechanical stirrer and a thermometer, heat up to 160°C, and slowly add 150g ...
example 2
[0025] 1) Add 44.1 g (0.28 mol) of o-chloronitrobenzene and 22.8 g (0.36 mol) of copper powder into a 500 mL three-neck round bottom flask equipped with a stirrer, a thermometer, and a reflux condenser. First heated to 220 ° C, and then maintain the temperature reaction 10h. Through chromatographic tracking detection, when the content of o-chloronitrobenzene in the raw material is lower than 2%, the temperature is lowered to stop the reaction, the reaction solution is cooled to room temperature, and 150 mL of dichloromethane is added to the reaction system for extraction. The reaction solution was washed with 450 mL*3 times of water, stirred to obtain a viscous solid, and then recrystallized through 200 mL of methanol. 51.2 g of light yellow solid 2,2-dinitrobiphenyl was obtained with a yield of 75%.
[0026] 2) Under the protection of an inert gas, put 48.8g (0.20mol) of 2,2-dinitrobiphenyl obtained in the above step into a 500mL three-necked reaction flask equipped with a m...
example 3
[0029] 1) Add 44.1 g (0.28 mol) of o-chloronitrobenzene and 19.7 g (0.31 mol) of copper powder into a 500 mL three-necked round bottom flask equipped with a stirrer, a thermometer, and a reflux condenser. The mixture was heated to 200 °C and kept for 10 h. Through chromatographic tracking detection, the reaction is stopped after the content of o-chloronitrobenzene in the raw material is less than 2%, cooled to room temperature, and 150 mL of dichloromethane is added to the reaction system for extraction. After hydrolysis, wash the reaction solution with 450mL*3 times of water, stir to obtain a viscous solid, and then recrystallize through 200mL of methanol. 52.6 g of light yellow solid 2,2-dinitrobiphenyl was obtained with a yield of 77%.
[0030] 2) Under the protection of an inert gas, put 48.8g (0.20mol) of 2,2-dinitrobiphenyl into a 500mL three-necked reaction flask equipped with a mechanical stirrer and a thermometer, raise the temperature to 150°C, and slowly add 150g (...
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