Novel preparation method of nitrogen heterocyclic perylene bisimide in bay area
A technology of perylene imide and alkyl tetrachloroperylene imide, which is applied in the field of preparation of novel nitrogen-heterocyclized perylene imide in the bay area, can solve the problems of unrealized synthesis, and achieve low cost and easy multiple production. The effect of functional modification and simple synthesis process
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Embodiment 1
[0021] Under argon, add 33.4 mg of alkyl tetrachloroperylene imide, 18.2 mg of 4-butoxyaniline, 5.1 mg of bis(tri-tert-butylphosphine) to a 50 ml schlenk reaction flask with magnetrons Palladium (0) and 77 mg of sodium tert-butoxide were added, and 2 ml of toluene was added, and the reaction was stirred at 105° C. for 12 hours. Cool to room temperature naturally, add 3 ml of water and 10 ml of dichloromethane for extraction, repeat three times, and combine the organic phases. Anhydrous sodium sulfate was added to dry for half an hour, filtered, and the solvent was recovered by distillation under reduced pressure. Using the mixed solvent of petroleum ether and dichloromethane with a volume ratio of 2:3 as the eluent, the mixture was separated by neutral silica gel column chromatography, the second band was collected, and the solvent was recovered by distillation to obtain an orange solid crude product. The crude product was recrystallized with a mixed solvent of dichloromethan...
Embodiment 2
[0023] Under argon, add 33.4 mg of alkyl tetrachloroperylene imide, 18.2 mg of 4-butoxyaniline, 5.1 mg of bis(tri-tert-butylphosphine) to a 50 ml schlenk reaction flask with magnetrons Palladium (0) and 77 mg of sodium tert-butoxide were added, and 2 ml of toluene was added, and the reaction was stirred at 105° C. for 22 hours. Cool to room temperature naturally, add 3 ml of water and 10 ml of dichloromethane for extraction, repeat three times, and combine the organic phases. Anhydrous sodium sulfate was added to dry for half an hour, filtered, and the solvent was recovered by distillation under reduced pressure. Using the mixed solvent of petroleum ether and dichloromethane with a volume ratio of 2:3 as the eluent, the mixture was separated by neutral silica gel column chromatography, the second band was collected, and the solvent was recovered by distillation to obtain an orange solid crude product. The crude product was recrystallized with a mixed solvent of dichloromethan...
Embodiment 3
[0025] Under argon, add 33.4 mg of alkyl tetrachloroperylene imide, 18.2 mg of 4-butoxyaniline, 5.1 mg of bis(tri-tert-butylphosphine) to a 50 ml schlenk reaction flask with magnetrons Palladium (0) and 77 mg of sodium tert-butoxide, and then 2 ml of toluene were added, and the reaction was stirred at 105° C. for 36 hours. Cool to room temperature naturally, add 3 ml of water and 10 ml of dichloromethane for extraction, repeat three times, and combine the organic phases. Anhydrous sodium sulfate was added to dry for half an hour, filtered, and the solvent was recovered by distillation under reduced pressure. Using the mixed solvent of petroleum ether and dichloromethane with a volume ratio of 2:3 as the eluent, the mixture was separated by neutral silica gel column chromatography, the second band was collected, and the solvent was recovered by distillation to obtain an orange solid crude product. The crude product was recrystallized with a mixed solvent of dichloromethane and...
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