Thiophenol fluorescent probe based on 7-lignocaine-3-hydroxycoumarin structure and preparation method thereof
A technology of hydroxycoumarin and diethylamino, applied in the direction of fluorescence/phosphorescence, chemical instruments and methods, luminescent materials, etc., can solve the problem of inability to selectively distinguish thiophenol and aliphatic thiol, and detect thiophenol It takes a long time to achieve the effect of easy monitoring and control, easy separation and high purity
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[0018] Example 1: Synthesis of 7-diethylamino-3-hydroxycoumarin. Dissolve 200.0mg (0.86mmol) of 7-diethylamino-3-aminocoumarin in 3mL of hydrochloric acid with a concentration of 1mol / L, heat up to 100°C, follow the reaction by TLC, and complete the reaction within 1.5 hours. Cool to room temperature and use 25 % Ammonia water was adjusted to neutral, and a large amount of yellow solid precipitated. Extract with 15 mL of dichloromethane each time, and extract three times. The organic phase was dried with anhydrous sodium sulfate, filtered, and the solvent was evaporated under reduced pressure. Silica gel column chromatography was separated and purified to obtain yellow Green solid 172.7mg, yield 86%. 1 HNMR(400MHz, CDCl 3 ): δ7.21(d,J=8.4Hz,1H), 6.99(s,1H), 6.63(s,1H), 6.56(s,1H), 5.80(s,1H) 3.40(q,J=6.8 Hz, 4H), 1.20 (t, J=6.8 Hz, 6H). 13 CNMR(100Hz, CDCl 3 ): δ160.7, 151.3, 147.9, 135.7, 126.8, 115.4, 109.3, 97.6, 44.2, 29.2, 11.9. HRMS (ESI) (C 13 H 15 NO 3 )m / z:calculatedfo...
Example Embodiment
[0019] Example 2: Synthesis of 7-diethylamino-3-hydroxycoumarin. Dissolve 200.0mg (0.86mmol) of 7-diethylamino-3-aminocoumarin in 3mL of 1.5mol / L hydrochloric acid, heat up to 100℃, follow the reaction by TLC, the reaction is complete in 1 hour, cool to room temperature, use 25% ammonia water was adjusted to neutral, and a large amount of yellow solid precipitated. Extract with 15 mL of dichloromethane each time, extract three times, dry the organic phase with anhydrous sodium sulfate, filter, evaporate the solvent under reduced pressure, and separate and purify by silica gel column chromatography. Yellow-green solid 184.7mg, yield 92%.
Example Embodiment
[0020] Example 3: Synthesis of 7-diethylamino-3-hydroxycoumarin. Dissolve 200.0mg (0.86mmol) of 7-diethylamino-3-aminocoumarin in 3mL1.5mol / L hydrochloric acid, heat up to 100℃, follow the reaction by TLC, the reaction is complete in 2 hours, cool to room temperature, use saturated carbonic acid The sodium hydrogen solution was adjusted to neutral, and a large amount of yellow solid was precipitated. Extract with 15 mL of dichloromethane each time, and extract three times. The organic phase was dried with anhydrous sodium sulfate, filtered, the solvent was evaporated under reduced pressure, and silica gel column chromatography was separated and purified. The yellow-green solid is 178.7mg, the yield is 89%.
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