A kind of fluorescent probe for detecting methanol and its application
A fluorescent probe and methanol technology, applied in the field of fluorescent probes, can solve the problems of complex measurement process and time-consuming, and achieve the effect of strong anti-interference and high sensitivity
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Embodiment 1
[0021] Synthesis of embodiment 1 rhodamine compound
[0022]
[0023] Rhodamine compound
[0024] Weigh 3-diethylaminophenol (1.65 g, 10.00 mmol) into a 100 mL flask, add 20 mL of toluene dried over molecular sieves, and stir slowly at 60°C until completely dissolved. Add phthalic anhydride (1.50 g, about 10.13 mmol) under N 2 Under protection, the mixture was refluxed for 12h. Adjust the pH to ≤4 with dilute hydrochloric acid solution (ω=20%) to obtain a purple-red precipitate. The product was suction-filtered, fully washed with distilled water, and dried to obtain 0.70 g of crude 4-diethylamino ketoacid, with a yield of 42.50%.
[0025] Weigh 1 g (3.2 mmol) of crude 4-diethylaminoketonic acid into a 100 mL flask, add 10 mL of methanesulfonic acid, stir at 50 °C until fully dissolved, add 0.4 g (3.80 mmol) of m-aminophenol, and N 2 Heated to 120°C under protection for 10 h. After the reaction was completed, cool to room temperature and wash with 0.1 M Na 2 CO 3 The...
Embodiment 2
[0026] Example 2 Synthesis of Probe 1
[0027]
[0028] Weigh 0.150 g (0.30 mmol) of the rhodamine compound prepared in Example 1 into a 50 ml flask, add 10 mL of 2.5 mol / L dilute hydrochloric acid solution, and stir thoroughly at room temperature. Place the flask in a mixture of ice and water with solid sodium chloride and stir for 5 min. Weigh NaNO 2 0.024 g (0.35 mmol) of the solid was slowly added to the reaction solution, and after being fully stirred for 20 min, 0.044 g (0.32 mmol) of p-nitroaniline was added to react for 20 min, and finally the pH was adjusted to neutral with 1 mol / L NaOH solution. The reaction solution was fully extracted with ethyl acetate (3 × 30 mL), the organic phases were combined, and washed with anhydrous MgSO 4 Fully dried, the solvent was evaporated under reduced pressure, and the column was chromatographed on silica gel (V 石油醚 :V 乙酸乙酯 =20:1), vacuum-dried to obtain probe 1 0.038g, yield 23.50%. 1 HNMR (400 MHz, CDCl 3 ) δ 8.26 (d, J...
Embodiment 3
[0029] Example 3 Synthesis of Probe 2
[0030]
[0031] According to the method of Example 2, 0.056 g of probe 2 was synthesized, with a yield of 43.33%. 1 H NMR (400 MHz, CDCl 3 )δ 8.05 (d, J = 7.4 Hz, 1H), 7.66 (dt, J = 23.3, 7.4 Hz, 2H), 7.45 (d, J = 8.6Hz, 2H), 7.38 (d, J = 8.7 Hz, 2H ), 7.30 (s, 1H), 7.24 (d, J = 7.4 Hz, 1H), 6.94 (d, J = 8.5 Hz, 1H), 6.77 (d, J = 8.5 Hz, 1H), 6.60 (d, J = 8.9 Hz, 1H),6.49 (s, 1H), 6.39 (d, J = 9.1 Hz, 1H), 3.39 (q, J = 7.0 Hz, 4H), 1.20 (t, J= 7.0 Hz, 6H). 13 C NMR (101 MHz, CDCl 3 ) δ 169.71, 153.11, 152.90, 152.73,149.65, 145.18, 144.83, 134.86, 131.92, 129.56, 129.35, 128.93, 127.24,124.96, 124.06, 120.72, 115.32, 112.04, 108.47, 104.97, 103.91, 97.55, 84.24,44.52, 37.12, 31.95, 29.73, 22.72, 14.16, 12.53. MS (ESI): [M+H + ] anal.calcdfor: C 30 h 25 ClN 4 o 3 :525.1687 ; found: 525.1692.
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