A kind of fluorine-containing probe and its preparation method and application
A probe and reaction technology, applied in the field of analytical chemistry, can solve problems such as poor anti-interference ability, cumbersome and complicated synthesis steps of probe molecules, and high cost
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0037] Another aspect of the embodiments of the present invention also provides the aforementioned method for preparing the fluorine-containing probe, which includes:
[0038] React the mixed reaction system comprising diamine, R-2-formylphenylboronic acid, and the first solvent at 0-100°C for 0.5-24h, then add a reducing agent to the mixed reaction system, and perform reduction at 0-50°C React for 1-6 hours to prepare the fluorine-containing probe.
[0039] In some more specific embodiments, the preparation method includes:
[0040] Dissolving diamine in the first solvent to form a solution, then adding R-2-formylphenylboronic acid to the obtained solution to form the mixed reaction system, and reacting at 0-100°C for 0.5-24h;
[0041] And, adding a reducing agent to the mixed reaction system in batches at 0-50° C., and then performing a reduction reaction at 0-50° C. for 1-6 hours to prepare the fluorine-containing probe.
[0042] Further, the time interval for adding the ...
Embodiment 1
[0087] Add ethylenediamine (67μL, 1.0mmol, 1.0equiv) into methanol (30mL), add 4-fluoro-2-formylphenylboronic acid (345mg, 2.05mmol, 2equiv) under stirring, stir at room temperature for 2h, and then The solution was placed in an ice bath and added sodium borohydride (116.6 mg, 3.07 mmol, 3 equiv) three times with an interval of 15 minutes. After adding sodium borohydride, the ice bath was removed, and the reaction was stirred at room temperature for 2 h; Obtain the first white solid, then add dichloromethane to dissolve the solid, then stir at room temperature for 1 h, centrifuge, and rotary evaporate to obtain the second white solid; finally dissolve the second white solid with 1mol / L sodium hydroxide solution, and then add concentrated The pH of the solution was adjusted to approximately 8 with hydrochloric acid, and a white precipitate was obtained. The precipitate was washed three times with ice water, and then dried in vacuum at 60° C. for 12 hours to obtain a fluorine-con...
Embodiment 2
[0096]Ethylenediamine (134μL, 2.0mmol, 1.0equiv) was added to methanol (30mL), and 4-(trifluoromethyl)-2-formylphenylboronic acid (876mg, 4.02mmol, 2equiv) was added under stirring. Stir and react at ℃ for 24h, then add potassium borohydride (318mg, 5.89mmol, 3equiv) to the solution three times in an ice bath with an interval of 30min, remove the ice bath after adding potassium borohydride, and then stir the reaction at 0°C 6h; after that, the first white solid was obtained by rotary evaporation, and then dichloromethane was added to dissolve the solid, and then stirred at room temperature for 6 hours, centrifuged and rotary evaporated to obtain the second white solid; finally, the second white solid was dissolved with 1mol / L potassium hydroxide solution. It was a white solid, and concentrated hydrochloric acid was added to adjust the pH of the solution to be approximately equal to 8 to obtain a white precipitate, which was washed three times with ice water, and then dried in v...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More