Resorufin-2, 4-dinitrodiphenyl ether and application of resorufin- 2, 4-dinitrodiphenyl ether to detection of thiophenol
A technology of dinitrophenyl ether and resorufin, which is applied in the field of the new compound resorufin-2,4-dinitrophenyl ether, which is used for the determination of thiophenol by ultraviolet-visible spectrophotometry, can solve the problem of operation Complicated, expensive, and inconvenient for popularization and application, etc., to achieve the effect of good selectivity, simple operation, and high accuracy
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Embodiment 1
[0018] Preparation of resorufin-2,4-dinitrophenyl ether
[0019] Add 0.15g (0.64mmol) resorufin sodium, 8mL dry DMF, 0.3mL triethylamine to a 25mL round bottom flask, stir at 40°C for 30 minutes, and dissolve 0.16g (0.79mmol) 2,4-dinitrochlorobenzene Dissolve in 2mL of dry DMF, then add dropwise into a round bottom flask, then add 0.1477g (0.90mmol) KI, stir at 80°C for 12 hours, after the reaction is complete, mix the solution with 50mL CH 2 Cl 2 Dilute, wash in sequence with distilled water (20mL×3), wash with brine (20mL×3), and dry under reduced pressure to obtain the crude product, which is purified by column chromatography, and the eluent is the volume ratio of ethyl acetate to petroleum ether For a 1:1 mixed solution, 0.1 g of yellow solid resorufin-2,4-dinitrophenyl ether was obtained, with a yield of 41%, and the structural formula was as follows
[0020]
[0021] Infrared spectra and 1 The H-NMR diagrams are shown in figure 1 and figure 2 , the specific spec...
Embodiment 2
[0025] The use of the compound resorufin-2,4-dinitrophenyl ether prepared in Example 1 in the detection of thiophenol, its specific detection method is as follows:
[0026] Add 4.5mL of absolute ethanol, 2.0mL of phosphate buffer solution with a pH value of 7.4, 0.05mL of 1.0mmol / L resorufin-2,4-dinitrophenyl ether to a 10mL colorimetric tube in sequence. Sulfone solution and the sample solution to be tested were fixed to volume with sub-boiling water, left to stand at room temperature for 20 minutes, and the absorbance of the reaction system was detected with a UV-visible spectrophotometer at a wavelength of 580nm, and calculated according to the formula A=0.01272C+0.01167 The concentration of thiophenol in the sample solution, where A is the absorbance value of the reaction system at 580nm, and C is the concentration of thiophenol in the reaction system, in μmol / L.
[0027] In order to prove the beneficial effects of the present invention, the inventor has carried out a larg...
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