Preparation method of a novel terbium complex probe and its use as a potassium ion recognition reagent
A technology of terbium complexes and compounds, applied in the field of new compounds, can solve problems such as insufficient accuracy, large ion interference, and many influencing factors
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Embodiment 1
[0057] Preparation of 4-bromomethylbenzophenone
[0058] In the reaction flask, add 19.6g (0.1mol) 4-methylbenzophenone, then add 100mLCCl 4 , stirred to dissolve, heated to reflux, and then kept under the irradiation of a high-pressure mercury lamp, added dropwise 16g (0.1mol) of bromine within 30min, and continued to stir and reflux for 2h after the addition. Then stop the reaction, remove part of the solvent by rotary evaporation to about 20-30mL, pour the mixture into 50mL of absolute ethanol, recrystallize, and filter to obtain 13.6g of white crystal 4-bromomethylbenzophenone, yield 49.4% , m.p.111-113°C. 1 HNMR (400MHz, CDCl 3 )δ(ppm)=4.54(s, 2H), 7.49(t, 2H, J=8Hz), 7.51(d, 2H, J=8Hz), 7.60(t, 1H, J=8Hz), 7.79(d, 2H, J=8Hz), 7.80(d, 2H, J=8Hz).
Embodiment 2
[0060] The preparation of compound Tb-L of the present invention
[0061] Step 1: Preparation of compound S2
[0062]
[0063] Dissolve 3.72g (13.59mmol) of 1,10-diaza-18-crown 6 in 78mL of 1,4-dioxane, and separately dissolve 3.06g (13.59mmol) of di-tert-butyl dicarbonate (BOC anhydride) In 42mL of 1,4-dioxane, add the BOC anhydride solution into the crown ether solution dropwise within 1.5h, stir at 40°C for 30min, then stir at room temperature for 16h. Then the solvent was removed by rotary evaporation, and the obtained crude product was purified by silica gel column chromatography (the eluent was CH 2 Cl 2 :CH 3 OH=80:20, TLC monitoring, iodine cylinder color development), to obtain 1946mg colorless oily liquid S2, yield 39.5%. 1 HNMR (400MHz, CDCl 3 )δ(ppm)=1.44(s, 9H), 2.83(t, 4H, J=5Hz), 3.51(t, 4H, J=6Hz), 3.60(bs, 12H), 3.64(t, 4H, J= 5Hz).
[0064] Step 2: Preparation of Compound S3
[0065]
[0066] 1946mg (5.37mmol) S2 and 2627mg (8.05mmol) Cs 2 CO ...
Embodiment 3
[0089] Compound of the invention from Example 2 Tb-L versus K + sensitivity test
[0090] In the following experiments, unless otherwise specified and pointed out, the solvent used in all recognition experiments is tertiary water. The concentration of compound Tb-L of the present invention is 8.0×10 -4 mol / L, the concentration of potassium ions is 0-30mM.
[0091] The specific method is: add 0.5mL of 8.0×10 -4 mol / L of the compound of the present invention, 0 μL, 5 μL, 10.5 μL, 16 μL, 21 μL, 26.5 μL, 32 μL, 37.5 μL, 44 μL, 51 μL, 60.5 μL, 72 μL, 84 μL, 95 μL, 105 μL, 115 μL, 125 μL, 137.5 μL, 150 μL 1.0mol / L KCl solution, dilute to 5mL. With 232nm as the excitation wavelength and a delay time of 0.2ms, the luminous intensity of the system at 545nm was obtained using a CaryEclipse fluorescence spectrophotometer. Utilize the ratio (I / I) of the luminous intensity under different potassium ion concentration conditions in the system to the luminous intensity when there is no p...
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