Preparation and application of a temperature-sensitive dual-fluorescent PDOTs based on single-arm TPE molecules
A temperature-sensitive, dual-fluorescence technology used in the field of biochemistry to solve problems such as less work
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Embodiment 1
[0049] 1) Preparation of monohydroxytetraphenylethylene (TPE-OH):
[0050] Dissolve 0.05 mol of 4-hydroxybenzophenone, 0.1 mol of Zn powder, and 0.05 mol of benzophenone in 150.0 mL of anhydrous THF, stir under a nitrogen atmosphere, and vacuumize for 30 min to keep the system dry and free of water. oxygen. Then slowly drop 0.27mol TiCl 4 , reacted in an ice bath for 30 min, and refluxed at 70 °C for 24 h under an argon atmosphere. After the reaction, the reactant was cooled to room temperature and injected with 10% K 2 CO 3 Aqueous solution quenched the reaction. After vacuum filtration with a sand core funnel paved with silica gel, the filtrate was obtained and extracted with ethyl acetate to separate the organic layer. Ethyl acetate was removed by rotary evaporation, and the resulting crude product was separated and purified by column chromatography (eluent: V 乙酸乙酯 :V 石油醚 =1:10) to obtain the initiator TPE-OH, vacuum-dried, the yield was 40%.
[0051] 2) Preparation...
Embodiment 2
[0065] According to the molar ratio of 1:2, take 4-hydroxybenzophenone and benzophenone respectively, and then take zinc powder and TiCl 4 , the molar weight of the zinc powder taken is 1.5 times the total molar weight of both the 4-hydroxybenzophenone and the benzophenone taken, and the TiCl 4The molar weight is 3 times of the total molar weight of 4-hydroxybenzophenone and benzophenone; 4-hydroxybenzophenone, benzophenone and zinc powder are dissolved in anhydrous tetrahydrofuran, Stir under a nitrogen atmosphere, vacuumize and circulate for 30 min to keep the system anhydrous and oxygen-free, then slowly add TiCl dropwise 4 , reacted in an ice bath for 30 min, under argon atmosphere, refluxed at 70 °C for 24 h; after the reaction was completed, cooled to room temperature, and added K with a mass fraction of 10% 2 CO 3 Aqueous solution, quenching reaction, extraction with ethyl acetate, rotary evaporation drying, obtains white crude product; Crude product crosses silica ge...
Embodiment 3
[0067] According to the molar ratio of 1:1.5, take 4-hydroxybenzophenone and benzophenone respectively, and then take zinc powder and TiCl 4 , the molar weight of the zinc powder taken is 1.25 times the total molar weight of both the 4-hydroxybenzophenone and the benzophenone taken, and the TiCl 4 The molar weight is 2.5 times of the total molar weight of 4-hydroxybenzophenone and benzophenone; 4-hydroxybenzophenone, benzophenone and zinc powder are dissolved in anhydrous tetrahydrofuran (without water THF), stirred under a nitrogen atmosphere, vacuum cycled for 30 min to keep the system anhydrous and oxygen-free, and then slowly added TiCl dropwise 4 , reacted in an ice bath for 30 min, under argon atmosphere, refluxed at 72 °C for 24 h; after the reaction was completed, cooled to room temperature, and added K 2 CO 3 Aqueous solution, quenching reaction, extraction with ethyl acetate, rotary evaporation drying, obtains white crude product; Crude product crosses silica gel c...
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