Method for synthesizing 1,2,3,4- tetradeutero-9-bromoanthracene
A synthetic method and a deuterium generation technology, applied in 1 field, can solve the problems of inability to carry out large-scale industrial production, high risk and cost, and complicated operation process, and achieve the effects of low cost, reduced production cost, and simple operation.
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Embodiment 1
[0021] 1) Add 148.1 grams (1 mole) of phthalic anhydride to a 3-liter four-neck flask, then add 92.6 grams (1.1 moles) of deuterated benzene, 1000 grams of dichloromethane and 133.3 grams (1 mole) of trichloro Aluminum chloride; the above reaction solution was stirred at room temperature for 3 hours. Filter, adjust the pH value of the water phase in the filtrate to about 10 with saturated sodium carbonate solution, separate the organic phase and the water phase after standing for stratification, add saturated sodium carbonate solution to the above organic phase for extraction 3 times, each time 300 grams, the organic phase was discarded, and the water phase was retained, then the pH value of the above water phase was adjusted to about 1-2 with concentrated hydrochloric acid, and then extracted 3 times with toluene, each time 300 grams. The above-mentioned extracted organic phase was dried with anhydrous sodium sulfate, and after filtration, the toluene was distilled off using ...
Embodiment 2
[0027] 1) Add 148.1 grams (1 mole) of phthalic anhydride to a 3-liter four-necked bottle, and then add 109.4 grams (1.3 moles) of deuterated benzene, 1000 grams of dichloromethane and 160 grams (1.2 moles) of trichloro Aluminum chloride; the above reaction solution was stirred at room temperature for 3 hours. Filter, adjust the pH value of the water phase in the filtrate to about 10 with 10% sodium hydroxide solution, separate the organic phase and the water phase after standing and layering, add 10% sodium hydroxide solution to the above organic phase to extract 3 times , 200 grams each time, discard the organic phase, keep the water phase, then adjust the pH value of the above water phase to about 1-2 with concentrated hydrochloric acid, and then extract 3 times with toluene, each time 300 grams. The above-mentioned extracted organic phase was dried with anhydrous sodium sulfate, and after filtration, the toluene was distilled off using a rotary evaporator to obtain 224.1 gr...
Embodiment 3
[0033] 1) Add 38 grams (0.256 moles) of phthalic anhydride to a four-necked flask, then add 32 grams (0.384 moles) of deuterated benzene, 200 grams of dichloromethane and 44 grams (0.333 moles) of aluminum trichloride ; The above reaction solution was stirred at room temperature for 3 hours. Filter, adjust the pH value of the water phase in the filtrate to about 10 with saturated sodium carbonate solution, separate the organic phase and the water phase after standing for stratification, add saturated sodium carbonate solution to the above organic phase for extraction 3 times, each time 100 grams, the organic phase was discarded, and the water phase was retained, then the pH value of the above water phase was adjusted to about 1-2 with concentrated hydrochloric acid, and then extracted with toluene 3 times, each time 100 grams. The above-mentioned extracted organic phase was dried with anhydrous sodium sulfate, and after filtration, the toluene was distilled off using a rotary ...
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