A kind of mercury ion optical probe and its preparation method and application
A technology of optical probes and mercury ions, applied in chemical instruments and methods, material analysis through optical means, organic chemistry, etc. Harsh conditions and other issues, to achieve the effect of strong anti-interference ability, high sensitivity, and easy preparation
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Embodiment 1
[0033] Weigh 239.5 mg of rhodamine B (0.5 mmol), dissolve it in 10 mL of 1,2-dichloroethane, add 0.3 mL of phosphorus oxychloride dropwise, and heat under reflux at 90 °C for 4 h. After the reaction was completed, the solvent was distilled off under reduced pressure to obtain a red rhodamine B acid chloride intermediate.
[0034] Weigh 52.1 mg N,N - Dimethylthiourea (0.5 mmol), which was dissolved in 5 mL of tetrahydrofuran, and 1.2 mL of triethylamine was added dropwise with stirring. The rhodamine B acid chloride prepared in the previous steps was dissolved in 5 mL of tetrahydrofuran, added dropwise to the above solution, and reacted at 20 °C for 10 h. After the reaction was completed, the solvent was distilled off under reduced pressure to obtain a purple-red substance, and then 10 mL of twice distilled water was added to it, extracted three times with dichloromethane (20 mL*3), and the solvent was distilled off under reduced pressure to obtain a crude product . The obta...
Embodiment 2
[0042]Weigh 239.5 mg of Rhodamine B (0.5 mmol), dissolve it in 12 mL of 1,2-dichloroethane, add 0.4 mL of phosphorus oxychloride dropwise, and heat to reflux at 95 °C for 5 h. After the reaction was completed, the solvent was distilled off under reduced pressure to obtain a red rhodamine B acid chloride intermediate.
[0043] Weigh 72.9 mg of N,N-dimethylthiourea (0.7 mmol), dissolve it in 6 mL of acetonitrile, and add 1.6 mL of triethylamine dropwise with stirring. The rhodamine B acid chloride prepared in the previous steps was dissolved in 5 mL of tetrahydrofuran, added dropwise to the above solution, and reacted at 35 °C for 5 h. After the reaction was completed, the solvent was distilled off under reduced pressure to obtain a purple-red substance, and 10 mL of twice distilled water was added to it, and extracted three times with dichloromethane (20 mL*3), and the solvent was distilled off under reduced pressure to obtain a crude product. The obtained crude product is sep...
Embodiment 3
[0045] Weigh 239.5 mg of rhodamine B (0.5 mmol), dissolve it in 13 mL of 1,2-dichloroethane, add 0.5 mL of phosphorus oxychloride dropwise, and heat under reflux at 100 °C for 5 h. After the reaction was completed, the solvent was distilled off under reduced pressure to obtain a red rhodamine B acid chloride intermediate.
[0046] Weigh 78.2 mg N,N - Dimethylthiourea (0.75 mmol), which was dissolved in 7 mL of acetonitrile, and 2.0 mL of triethylamine was added dropwise with stirring. The rhodamine B acid chloride prepared in the previous steps was dissolved in 5 mL of acetonitrile, added dropwise to the above solution, and reacted at 10 °C for 12 h. After the reaction was completed, the solvent was distilled off under reduced pressure to obtain a purple-red substance, and then 10 mL of double-distilled water was added to it, and extracted three times with dichloromethane (20 mL*3), and the solvent was distilled off under reduced pressure to obtain a crude product. The obtai...
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