A kind of oxazole drug molecule used for hospital sterilization and its preparation method
A technology of drug molecules and oxazoles is applied in the field of antibacterial drug synthesis to achieve good antibacterial effect.
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Embodiment 1
[0022]
[0023] In a reaction flask with a stirrer, add 13g of p-tolueneacetonitrile and 6.5g of ZSM-5 molecular sieve into 60g of N,N-dimethylformamide dimethyl acetal, and slowly raise the temperature under the protection of nitrogen To 70°C, TLC monitors that the reaction of p-tolueneacetonitrile is complete, after cooling down to room temperature, add 120mL of ethanol and 100mL of water to the reaction system, cool down to about 10°C again, stir for 20min, filter the reaction solution, concentrate the reaction solution, and then add to the reaction system 50 mL of ethyl acetate was added to the liquid, the organic phase was separated, the aqueous phase was extracted several times with 50 mL of ethyl acetate, the organic phases were combined and concentrated to obtain 2-(4-methylphenyl)-3-(dimethylamino) -Acrylonitrile; Add 14g of 2-(4-methylphenyl)-3-(dimethylamino)-acrylonitrile and potassium carbonate to 150mL of ethanol, and slowly add it dropwise under nitrogen prote...
Embodiment 2
[0025] In a reaction flask with a stirrer, add 13g of p-tolueneacetonitrile and 1.3g of ZSM-5 molecular sieve into 50g of N,N-dimethylformamide dimethyl acetal, and slowly raise the temperature under the protection of nitrogen To 70°C, TLC monitors the complete reaction of p-tolueneacetonitrile, after cooling down to room temperature, add 100mL of ethanol and 100mL of water to the reaction system, lower the temperature to about 10°C again, stir for 20min, filter the reaction solution, concentrate the reaction solution, and add to the reaction system 50 mL of ethyl acetate was added to the liquid, the organic phase was separated, the aqueous phase was extracted several times with 50 mL of ethyl acetate, the organic phases were combined and concentrated to obtain 2-(4-methylphenyl)-3-(dimethylamino) -Acrylonitrile; Add 14g of 2-(4-methylphenyl)-3-(dimethylamino)-acrylonitrile and potassium carbonate to 150mL of ethanol, and slowly add it dropwise under nitrogen protection at room...
Embodiment 3
[0027]
[0028] In a reaction flask with a water separator, add 13g of p-tolueneacetonitrile, 11g of sodium methoxide and 9g of ethyl formate into 100mL of toluene, and slowly raise the temperature to reflux under the protection of nitrogen. Then the reaction was lowered to room temperature, and the reaction was continued until TLC monitored that the raw materials were completely reacted. Add 100 mL of water to the reaction system, and then use 20% hydrochloric acid to adjust the pH of the reaction solution to 3-4. A large amount of solids precipitated, and suction filtered The reaction solution and the filter cake were dried to obtain 2-(4-methylphenyl)-2-nitrile-acetaldehyde (melting point was 152~154°C); the obtained 2-(4-methylphenyl)-2 Add 12 g of nitrile-acetaldehyde and potassium tert-butoxide to 100 mL of ethanol. Under nitrogen protection, at room temperature, slowly add 50 mL of an ethanol solution in which 7 g of hydroxylamine hydrochloride is dissolved, and contr...
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