Oxazole-linked triazole drug molecule for sterilization and disinfection, and preparation method and application thereof
A technology of drug molecules and triazoles, used in antibacterial drugs, organic chemistry and other directions to achieve good antibacterial effect
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Embodiment 1
[0024]
[0025] In a reaction flask with a water separator, add 12g of 4-methylbenzaldehyde, 11g of sodium methoxide and 12g of anhydrous magnesium sulfate into 24g of acetone and 200mL of benzene, slowly raise the temperature to reflux, and pass through the water separator during the reflux reaction Drain the moisture generated in the reaction process. After 7 hours of reaction, TLC monitors the reaction of the raw materials completely. Filter the reaction solution, pour the filtrate into 250 mL of water, adjust the pH of the reaction solution with dilute hydrochloric acid to be neutral, and then extract 3 times with 50 mL of dichloromethane. The organic phases were combined, separated and purified by silica gel column chromatography to obtain 7.8 g of 4-(p-tolyl)-3-buten-2-one; LC-MS (ESI): m / z 161 [M+H] + ; 1 H NMR (400MHz, CDCl 3 ): δ7.49(d, J=16.0Hz, 1H), 7.42(d, J=8.0Hz, 2H), 7.19(d, J=8.0Hz, 2H), 6.70(d, J=16.0Hz, 1H ), 2.36(s,3H), 1.83(s,3H).
Embodiment 2
[0027]In a reaction flask with a water separator, add 12g of 4-methylbenzaldehyde, 17g of potassium hydroxide and 12g of anhydrous magnesium sulfate into 12g of acetone and 200mL of benzene, and slowly raise the temperature to reflux. The water produced during the reaction was discharged from the reactor, and the reaction solution was filtered after 3 hours of reaction, and the filtrate was poured into 250 mL of water, and the pH of the reaction solution was adjusted to be neutral by dilute hydrochloric acid, then extracted 3 times with 50 mL of dichloromethane, combined the organic phases, and then Separation and purification by silica gel column chromatography yielded 5.9 g of 4-(p-tolyl)-3-buten-2-one; LC-MS (ESI): m / z 161 [M+H] + ; 1 H NMR (400MHz, CDCl 3 ): δ7.49(d, J=16.0Hz, 1H), 7.42(d, J=8.0Hz, 2H), 7.19(d, J=8.0Hz, 2H), 6.70(d, J=16.0Hz, 1H ), 2.36(s,3H), 1.83(s,3H).
Embodiment 3
[0029] In a reaction flask with a water separator, add 12g of 4-methylbenzaldehyde, 11.5g of potassium methylate and 12g of anhydrous magnesium sulfate into 24g of acetone and 200mL of benzene, and slowly raise the temperature to reflux. The water generated in the reaction process was discharged from the reactor, and the reaction solution was filtered after 4.5 hours of reaction, the filtrate was poured into 250 mL of water, the pH of the reaction solution was adjusted to be neutral by dilute hydrochloric acid, and then extracted 3 times with 50 mL of dichloromethane, and the organic phases were combined. Then separated and purified by silica gel column chromatography to obtain 10.1 g of 4-(p-tolyl)-3-buten-2-one, LC-MS (ESI): m / z 161 [M+H] + ; 1 H NMR (400MHz, CDCl 3 ): δ7.49(d, J=16.0Hz, 1H), 7.42(d, J=8.0Hz, 2H), 7.19(d, J=8.0Hz, 2H), 6.70(d, J=16.0Hz, 1H ), 2.36(s,3H), 1.83(s,3H).
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