Preparation method of metal complex fluorescence probe for detecting hydrogen sulfide and application thereof
A metal complex and fluorescent probe technology, applied in the field of analytical chemistry, to achieve the effects of good selectivity, good sensitivity analysis, and good photostability
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[0027] Example 1
[0028] A preparation method of a metal complex fluorescent probe, the method steps are as follows:
[0029] S1: Add 0.1 g of dansyl chloride and 80 μL of triethylamine to a round-bottomed flask containing 8 mL of dichloromethane, then add 0.0043 g of chloroethylamine hydrochloride, and under the protection of nitrogen, the reaction is stirred at room temperature for 0.5 h , the dichloromethane solvent was removed with a rotary evaporator to obtain a yellow oil;
[0030] S2: The resulting material was then subjected to a silica gel column in petroleum ether:ethyl acetate=4:1, R f =0.42 under the condition of separation and purification to obtain the product Ds-1;
[0031] S3: Weigh 0.06g of Ds-1 product and place it in 2mL of DMF to dissolve, then add 0.03g of furan-2-ylmethyl-pyridin-2-ylmethyl-amine and 0.02g of anhydrous potassium carbonate, stir at room temperature for 22h Then, 12 mL of ice water was added to the reaction mixture, a large amount of pr...
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[0033] Example 2
[0034] S1: Add 0.1500g of dansyl chloride and 117μL of triethylamine into a round-bottomed flask containing 10mL of dichloromethane, then add 0.0065g of chloroethylamine hydrochloride, and under the protection of nitrogen, the reaction is stirred at room temperature for 1h, The dichloromethane solvent was removed with a rotary evaporator to obtain a yellow oil;
[0035] S2: The resulting material was then subjected to a silica gel column in petroleum ether:ethyl acetate=4:1, R f =0.42 under the condition of separation and purification to obtain the product Ds-1;
[0036] S3: Weigh 0.0625g of Ds-1 product and place it in 3mL of DMF to dissolve, then add 0.0376g of furan-2-ylmethyl-pyridin-2-ylmethyl-amine and 0.0276g of anhydrous potassium carbonate, stir at room temperature for 24h Then, 15 mL of ice water was added to the reaction mixture, a large amount of precipitation was formed, and the solid precipitate was obtained by filtration, and then the obtain...
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[0038] Example 3
[0039] S1: Add 0.2 g of dansyl chloride and 160 μL of triethylamine into a round-bottomed flask containing 12 mL of dichloromethane, then add 0.0086 g of chloroethylamine hydrochloride, and under the protection of nitrogen, the reaction is stirred at room temperature for 1.5 h , the dichloromethane solvent was removed with a rotary evaporator to obtain a yellow oil;
[0040] S2: The resulting material was then subjected to a silica gel column in petroleum ether:ethyl acetate=4:1, R f =0.42 under the condition of separation and purification to obtain the product Ds-1;
[0041] S3: Weigh 0.07g of Ds-1 product and place it in 4mL of DMF to dissolve, then add 0.04g of furan-2-ylmethyl-pyridin-2-ylmethyl-amine and 0.04g of anhydrous potassium carbonate, stir at room temperature for 26h Then, 18 mL of ice water was added to the reaction mixture, a large amount of precipitation was formed, and the solid precipitate was obtained by filtration, and then the obtaine...
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