V-type coumarin fluorescent probe for hydrazine hydrate detection and preparation method thereof
A fluorescent probe, coumarin technology, applied in fluorescence/phosphorescence, chemical instruments and methods, luminescent materials, etc., can solve the problems of limited number of fluorescent probes, influence of interfering ions, complex probe synthesis, etc., to prevent interference , the effect of simple synthesis and low cost
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Embodiment 1
[0028] (1) Dissolve 13 mmol of diethyl malonate and 5 mmol of salicylaldehyde in 20 mL of ethanol, add dropwise two drops of glacial acetic acid and 0.1 mL of piperidine, and stir under reflux for 6 h at room temperature; add ice water after the reaction is complete A precipitate was precipitated, filtered and washed with ice water to obtain ethyl coumarin-3-carboxylate as a white solid;
[0029] (2) Mix 5 mmol of ethyl coumarin-3-carboxylate and 2.5 mmol of resorcinol, add 0.02 g of DMAP, and 2 Heated to 140°C under protection, reacted for 3 h, added ethanol and sonicated for 10 min, filtered and rinsed with ethanol to obtain V-type coumarin in the form of orange-yellow solid;
[0030] (3) Mix and dissolve 5 mmol V-type coumarin and 7 mmol 4-fluorobutyric acid in 20 mL of dichloromethane, add 0.02 g DMAP and 0.2 g DCC, stir at room temperature for 4 h, and distill off the solvent under reduced pressure The crude probe was obtained and purified by column chromatography with d...
Embodiment 2
[0032] (1) Dissolve 13 mmol of diethyl malonate and 5 mmol of salicylaldehyde in 20 mL of ethanol, add dropwise two drops of glacial acetic acid and 0.1 mL of piperidine, and stir at room temperature for 8 h under reflux; after the reaction is complete, add ice water A precipitate was precipitated, filtered and washed with ice water to obtain ethyl coumarin-3-carboxylate as a white solid;
[0033] (2) Mix 5 mmol of ethyl coumarin-3-carboxylate and 2.5 mmol of resorcinol, add 0.02 g of DMAP, and 2 Heated to 140°C under protection, reacted for 4 h, added ethanol and sonicated for 15 min, filtered and rinsed with ethanol to obtain V-type coumarin in the form of orange-yellow solid;
[0034] (3) Mix and dissolve 5 mmol V-type coumarin and 7 mmol 4-chlorobutyric acid in 20 mL of dichloromethane, add 0.02 g DMAP and 0.2 g DCC, stir at room temperature for 6 h, and distill off the solvent under reduced pressure The crude probe was obtained and purified by column chromatography with ...
Embodiment 3
[0036] (1) Dissolve 13 mmol of diethyl malonate and 5 mmol of salicylaldehyde in 20 mL of ethanol, add dropwise two drops of glacial acetic acid and 0.1 mL of piperidine, and stir under reflux for 6 h at room temperature; add ice water after the reaction is complete A precipitate was precipitated, filtered and washed with ice water to obtain ethyl coumarin-3-carboxylate as a white solid;
[0037] (2) Mix 5 mmol of ethyl coumarin-3-carboxylate and 2.5 mmol of resorcinol, add 0.1 g of AlCl 3 , at N 2 Heated to 140°C under protection, reacted for 3 h, added ethanol and sonicated for 10 min, filtered and rinsed with ethanol to obtain V-type coumarin in the form of orange-yellow solid;
[0038] (3) Mix and dissolve 5 mmol V-type coumarin and 7 mmol 4-chlorobutyric acid in 20 mL of dichloromethane, add 0.02 g DMAP and 0.2 g DCC, stir at room temperature for 5 h, and distill off the solvent under reduced pressure The crude probe was obtained and purified by column chromatography wi...
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