Synthesis and application of a near-infrared fluorescent probe for detecting hydrogen sulfide
A fluorescent probe and near-infrared technology, applied in the field of fluorescent probe sensing in analytical chemistry, can solve the problems of inability to accurately measure hydrogen sulfide content, complicated instrument measurement operations, complex components, etc., and achieve low biological damage and selectivity. Good, easy to synthesize effects
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Embodiment 1
[0020] Ethyl acetoacetate (3.17g, 24mmol) and diethylamino salicylaldehyde (3.77g, 19.5mmol) were dissolved in 20ml of ethanol, 3 drops of piperidine were added dropwise, and the mixture was stirred and refluxed for 10 hours. Stop the reaction, cool to room temperature, filter to obtain a bright yellow precipitate, and wash once with ice-free ethanol (5 ml). Recrystallized from absolute ethanol to obtain 7-diethylaminobenzopyrone (4.74 g of yellow solid, yield 91.4%). In a 25ml three-necked flask, 8ml DMF was cooled and stirred at 5°C, and POCl was slowly added dropwise through a constant pressure funnel 3 (3.5ml, 23.0mmol) (keep the temperature at 5°C), slowly add compound 1 (1g, 3.9mmol), the reaction was stirred at 5°C for 3h, then reacted at room temperature for 2h, transferred to an oil bath and heated at 80°C for reaction 7h. Stop the reaction, cool to room temperature, add dropwise into crushed ice for deep cooling, neutralize pH=8 with sodium carbonate (the process k...
Embodiment 2
[0022] Ethyl acetoacetate (2.0g, 15.1mmol) and diethylamino salicylaldehyde (1.93g, 10mmol) were dissolved in 15ml of ethanol, 5 drops of piperidine were added dropwise, and the mixture was stirred and refluxed for 8 hours. Stop the reaction, cool to room temperature, filter to obtain a bright yellow precipitate, and wash once with 8 ml ice-free ethanol. Recrystallized from absolute ethanol to obtain 7-diethylaminobenzopyrone (yellow solid 2.31 g, yield 89.1%). In a 25ml three-necked flask, 6ml of DMF was cooled and stirred at 0°C, and POCl was slowly added dropwise through a constant pressure funnel 3 (4.7ml, 30.9mmol) (keep the temperature at 0°C), slowly add compound 1 (1.5g, 5,85mmol), the reaction was stirred at 0°C for 4h, then reacted at room temperature for 4h, transferred to an oil bath and heated for 75 ℃ reaction 8h. Stop the reaction, cool to room temperature, add dropwise into crushed ice for deep cooling, neutralize pH=7 with sodium carbonate (keep the temperat...
Embodiment 3
[0024] Ethyl acetoacetate (1.5g, 11.25mmol) and diethylamino salicylaldehyde (2.17g, 11.25mmol) were dissolved in 10ml of ethanol, 4 drops of piperidine were added dropwise, and the mixture was stirred and refluxed for 10 hours. Stop the reaction, cool to room temperature, filter to obtain a bright yellow precipitate, and wash once with 10 ml ice-free ethanol. Recrystallized from absolute ethanol to obtain 7-diethylaminobenzopyrone (yellow solid 1.8 g, yield 61.7%). In a 25ml three-necked flask, 10ml of DMF was cooled and stirred at -5°C, and POCl was slowly added dropwise through a constant pressure funnel 3 (2.3ml, 15mmol) (keep the temperature at -5°C), slowly add compound 1 (1.8g, 7.02mmol), the reaction was stirred at -5°C for 6h, then reacted at room temperature for 3h, transferred to an oil bath and heated for 90 ℃ reaction 11h. Stop the reaction, cool to room temperature, drop into crushed ice for deep cooling, neutralize pH=9 with sodium carbonate (the process keeps...
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