Rapid detection reagent kit for benzoyl peroxide
A technology of benzoyl peroxide and reagents, which is applied in material analysis through observation of the influence of chemical indicators, analysis through chemical reactions of materials, organic chemistry, etc., to achieve mild reaction, great application prospects, and excellent performance Effect
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Embodiment 1
[0041] The preparation of the phenylboronic ester compound containing resorufin fluorophore shown in embodiment 1, formula I
[0042] Dissolve 7-hydroxyphenoxazinone sodium salt (1mmol) in DMF (10mL), add 2-bromomethylphenylboronic acid pinacol ester (1mmol), catalyst potassium carbonate (1mmol) in the reaction solution, and React at 30°C for 1 hour. After the reaction was completed, after cooling, the solvent was concentrated under reduced pressure to obtain a crude product, which was purified by column chromatography using n-hexane / ethyl acetate (2:1, v / v) as eluent to obtain 250 mg of the product.
[0043] The structural characterization data results of the product are as follows: 1 H NMR (300MHz, CDCl 3 )δ(ppm): 7.92(d, 1H, J=7.3Hz), 7.74(d, 1H, J=8.9Hz), 7.48(m, 3H), 7.39(m, 1H), 7.05(m, 1H) , 6.98(d, 1H, J=2.5Hz), 6.91(d, 1H, J=9.8Hz), 6.46(s, 1H), 5.48(s, 2H), 1.29(s, 12H); 13 C NMR (75MHz, CDCl 3 )δ(ppm): 186.3, 163.4, 149.9, 145.7, 145.3, 141.5, 136.4, 134.7, 134...
Embodiment 2
[0045] Embodiment 2, the preparation of the phenylboronic ester compound containing resorufin fluorophore shown in formula I
[0046] Dissolve 7-hydroxyphenoxazinone sodium salt (1mmol) in DMF (10mL), add 2-bromomethylphenylboronic acid pinacol ester (4mmol), catalyst potassium carbonate (4mmol) in the reaction solution, and in React at 0-5°C for 24 hours. After the reaction was completed, after cooling, the solvent was concentrated under reduced pressure to obtain a crude product, which was purified by column chromatography using n-hexane / ethyl acetate (2:1, v / v) as eluent to obtain 200 mg of the product.
[0047] The structural characterization data results of the product are as follows: 1 H NMR (300MHz, CDCl 3 )δ(ppm): 7.92(d, 1H, J=7.3Hz), 7.74(d, 1H, J=8.9Hz), 7.48(m, 3H), 7.39(m, 1H), 7.05(m, 1H) , 6.98(d, 1H, J=2.5Hz), 6.91(d, 1H, J=9.8Hz), 6.46(s, 1H), 5.48(s, 2H), 1.29(s, 12H); 13 C NMR (75MHz, CDCl 3 )δ(ppm): 186.3, 163.4, 149.9, 145.7, 145.3, 141.5, 136.4, 134....
Embodiment 3
[0049] Embodiment 3, the benzoyl peroxide concentration in the semi-quantitative determination sample with kit
[0050] The concentration of benzoyl peroxide in the sample is semi-quantitatively determined by the kit, which is determined according to the following steps:
[0051] 1) Weigh 242 mg of benzoyl peroxide, dissolve it in 100 mL of ethanol, and prepare a 10 mM standard stock solution of benzoyl peroxide.
[0052] 2) In the sample bottle, add 2.5mL of reagent stock solution 1 and 9 μL of reagent stock solution 2 in sequence, then add the appropriate volume of benzoyl peroxide standard stock solution prepared in step 1), dilute to 3mL with water and ethanol, and make The final concentrations of benzoyl peroxide were: (a) 0 μM; (b) 1 μM; (c) 10 μM; (d) 30 μM; (e) 60 μM; (f) 100 μM. A series of color rendering standards, such as figure 1 As shown in a-f, from a-f, the color of the solution gradually deepens from the color of the solvent itself to deep pink.
[0053] Wh...
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