Synthesis of multi-signal fluorescent probe and application of multi-signal fluorescent probe in simultaneously distinguishing Cys, SO2, GSH and Hcy
A technology of fluorescent probes and fluorescent molecular probes, applied in the field of analytical chemistry, can solve the problem that thiol fluorescent probes cannot be distinguished and detected by four channels at the same time
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Embodiment 1
[0027] Example 1. Synthesis of 4-hydroxy-7-(pyrrolidin-1-yl)-2H-chromen-2-one
[0028] a. Diphenylmalonate (6.28 g, 24.51 mmol) and 3-(pyrrolidin-1-yl)phenol (2 g, 12.25 mmol) were added to anhydrous toluene (20 mL), and the reaction mixture was heated to 110 ℃ for 8 hours,
[0029] b. After the reaction is completed, filter, wash the filter cake 3 times with n-hexane, and dry in vacuo to obtain light yellow solid 4-hydroxy-7-(pyrrolidin-1-yl)-2H-chromen-2-one (2.0 g, 68% yield).
Embodiment 2
[0030] Example 2. Synthesis of 4-chloro-2-oxo-7-(pyrrolidin-1-yl)-2H-methylene-3-carbaldehyde
[0031] . Under nitrogen protection, slowly add 1.8 mL of dry redistilled N,N-dimethylformamide (DMF) to an equal volume of phosphorus oxychloride (POCl 3 ), stirred at 20-50°C for 30 minutes to obtain a red solution,
[0032] . 4-Hydroxy-7-(pyrrolidin-1-yl)-2H-chromen-2-one (1.0 g, 4.32 mmol) was dissolved in 5 mL N,N-dimethylformamide and added dropwise to step In the mixed solution, the mixture continued to stir and react at 60°C under nitrogen protection for 12 hours,
[0033] . After the reaction is complete, the step Slowly pour the reaction solution in 500 mL of ice water, adjust the pH to 6 with 20% NaOH solution, a large amount of precipitation occurs, filter, wash the filter cake with an appropriate amount of deionized water for 3 times, and dry the obtained solid in vacuum to obtain 4-chloro -2-Oxo-7-(pyrrolidin-1-yl)-2H-methylene-3-carbaldehyde
[0034] 0.74...
Embodiment 3
[0035] Example 3. Synthesis of 4-(butylthio)-2-oxo-7-(pyrrolidin-1-yl)-2H-methylene-3-carbaldehyde
[0036] . Add 0.20 g (720.19 mmol) of 4-chloro-2-oxo-7-(pyrrolidin-1-yl)-2H-methylene-3-carbaldehyde and 64.95 mg (720.19 mmol) of n-butanethiol to 20 mL In anhydrous dichloromethane, add 70 μL triethylamine dropwise, and stir the reaction at room temperature.
[0037] . After the reaction is complete, the step 4-(butylthio)-2-oxo-7-(pyrrolidin-1-yl)-2H-methylene-3-carbaldehyde was obtained by column chromatography of the reaction solution.
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