Based on triaryl phosphorus oxy compound and its preparation method and application
A technology of oxygen compounds and triarylphosphorus, which is applied in the field of triarylphosphorus oxides and its preparation, can solve the problems of low fluorescence quantum yield, high production cost, and small detection range, and achieve simple synthesis, high decomposition temperature, and stable good sex effect
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Embodiment 1
[0037] Preparation of diphenyl(1'-pyrene)phosphorus oxide
[0038] Experimental steps:
[0039] (1) Under the protection of nitrogen, 1-bromopyrene (2g, 7.6mmol, 1equiv) was dissolved in dry ether, cooled in a dry ice acetone bath (-78°C), and n-butyllithium (5ml, 7.6mmol, 1equiv), after stirring for 2 hours, remove the dry ice acetone bath and heat up to normal temperature and react for 1 hour.
[0040] (2) After the reaction was completed, diphenylphosphorous chloride (1.71 g, 7.6 mmol, 1 equiv) was added dropwise to the reaction system, and the reaction was continued for 8 hours under nitrogen protection. After the reaction, the organic phase was extracted, combined and concentrated to dryness to obtain a solid.
[0041] (3) The obtained solid was dissolved in dichloromethane, and hydrogen peroxide (H 2 o 2 ) (0.17g, 15.2mmol, 2equiv), stirred for 3 hours. After the reaction, the organic phase was extracted, combined and concentrated, and separated and purified by a ch...
Embodiment 2
[0043] Preparation of diphenyl(1'-pyrene)phosphorus oxide
[0044] Experimental steps:
[0045] (1) Under the protection of nitrogen, 1-bromopyrene (2g, 7.6mmol, 1equiv) was dissolved in dry ether, cooled in a dry ice acetone bath (-78°C), and n-butyllithium (6ml, 9.1mmol, 1.2equiv), after stirring for 2 hours, the dry ice acetone bath was removed and the temperature was raised to normal temperature for reaction for 1 hour.
[0046] (2) After the reaction, diphenylphosphorus chloride (1.14 g, 5.1 mmol, 0.67 equiv) was added dropwise to the reaction system, and the reaction was continued for 6 hours under nitrogen protection. After the reaction, the organic phase was extracted, combined and concentrated to dryness to obtain a solid.
[0047] (3) The obtained solid was dissolved in dichloromethane, and hydrogen peroxide (H 2 o 2 ) (0.17g, 15.2mmol, 2equiv), stirred for 3 hours. After the reaction, the organic phase was extracted, combined and concentrated, and separated and...
Embodiment 3
[0049] Preparation of phenylbis(1'-pyrene)phosphorus oxide
[0050] Experimental steps:
[0051] (1) Under the protection of nitrogen, 1-bromopyrene (1g, 3.8mmol, 2equiv) was dissolved in dry ether, cooled in a dry ice acetone bath (-78°C), and n-butyllithium (2.5ml , 3.8mmol, 2equiv), after stirring for 2 hours, the dry ice acetone bath was removed and the temperature was raised to normal temperature to react for 1 hour.
[0052] (2) After the reaction was completed, phenylphosphorus dichloride (0.34 g, 1.9 mmol, 1 equiv) was added dropwise to the reaction system, and the reaction was continued for 8 hours under nitrogen protection. After the reaction, the organic phase was extracted, combined and concentrated to dryness to obtain a solid.
[0053] (3) The obtained solid was dissolved in dichloromethane, and hydrogen peroxide (H 2 o 2 ) (0.043g, 3.8mmol, 2equiv), stirred for 5 hours. After the reaction, the organic phase was extracted, combined and concentrated, and sepa...
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