A kind of fluorescent compound and its preparation method and the method and application of using the fluorescent compound to prepare sensing thin film
A fluorescent compound and compound technology, applied in steroids, fluorescence/phosphorescence, chemical instruments and methods, etc., can solve problems such as hindering practical application, non-reusable, poor film assembly performance, etc., achieving fully reversible detection and long service life. Long and stable effect
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[0036] The preparation method of fluorescent compound of the present invention comprises the following steps:
[0037] 1. Preparation of compound 5 (for details, refer to the Chinese invention patent with publication number CN102604140A)
[0038] ①Synthesis of 2,5-diiodo-1,4-bis(methoxy)-benzene
[0039] Under the protection of nitrogen, add iodine, potassium iodate and a mixture of water and concentrated sulfuric acid to the acetic acid solution of p-methoxybenzene respectively; react at 80°C for 8-12 hours, filter with suction, and dry in vacuum to obtain a white solid, namely 2 ,5-Diiodo-1,4-bis(methoxy)-benzene. Wherein, the molar ratio of p-methoxybenzene, iodine, potassium iodate, water and concentrated sulfuric acid is 1:(0.8-1.2):(0.2-0.6):(150-190):(1-3). Its reaction equation is as follows:
[0040]
[0041] ②Synthesis of 2,5-diiodo-1,4-di(hydroxyl)-benzene
[0042] Under nitrogen protection, 2,5-diiodo-1,4-bis(methoxy)-benzene was dissolved in dichloromethane...
Embodiment 1
[0085] 1. Preparation of fluorescent compounds containing cholesterol and sugar structures
[0086] ①Synthesis of 2,5-diiodo-1,4-bis(methoxy)-benzene
[0087] Under nitrogen protection, 2.0 g of p-methoxybenzene, 4.0 g of iodine, 1.22 g of potassium iodate and 15 mL of 10% sulfuric acid aqueous solution were added to 140 mL of acetic acid solution. After stirring at 80°C for 10 hours, the resulting large amount of solid was suction-filtered and dried in vacuo to obtain a white solid, namely 2,5-diiodo-1,4-bis(methoxy)-benzene. The molar ratio of p-methoxybenzene, iodine, potassium iodate, acetic acid and concentrated sulfuric acid is 1:1:0.4:170:2;
[0088] ②Synthesis of 2,5-diiodo-1,4-di(hydroxyl)-benzene
[0089] Under the protection of nitrogen, 7.8g of 2,5-diiodo-1,4-di(methoxy)-benzene was dissolved in 50mL of dichloromethane, and 5.58mL of Tris boron bromide. After the dropwise addition was completed, the mixture was stirred at room temperature for 16 hours, and a la...
Embodiment 2
[0121] ①Synthesis of 2,5-diiodo-1,4-bis(methoxy)-benzene
[0122] Under nitrogen protection, 2.0 g of p-methoxybenzene, 3.2 g of iodine, 1.22 g of potassium iodate and 15 mL of 10% sulfuric acid aqueous solution were added to 140 mL of acetic acid solution, and stirred at 80°C for 10 hours. The resulting large amount of solid was suction filtered and dried in vacuo to obtain a white solid. The molar ratio of p-methoxybenzene, iodine, potassium iodate, acetic acid and concentrated sulfuric acid is 1:0.8:0.4:170:2;
[0123] ② into 2,5-diiodo-1,4-di(hydroxyl)-benzene
[0124] Under nitrogen protection, 7.8g of 2,5-diiodo-1,4-bis(methoxy)-benzene was dissolved in 50mL of dichloromethane, and 3.72mL of Tris boron bromide. A large amount of solid produced was suction-filtered and dried in vacuo to obtain a white solid, namely 2,5-diiodo-1,4-bis(hydroxyl)-benzene. The molar ratio of 2,5-diiodo-1,4-bis(methoxy)-benzene, boron tribromide and dichloromethane is 1:2:40;
[0125] ③ S...
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