A kind of antibacterial agent and its synthesis method and application
A synthesis method and technology of antibacterial agents, applied in the field of antibacterial agents and their synthesis, can solve the problems of low content, complex extraction and purification process, high production cost, etc., and achieve the effects of high product purity, high product yield, and convenient operation
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[0023] The synthesis method of the antibacterial agent of the present embodiment may comprise the following steps: 2,6-dimethoxymethoxyacetophenone, 3,4,5-trimethoxymethoxybenzaldehyde and dehydrated alcohol are added to the round bottom The flask was mixed in an ice-water bath to obtain the first mixed solution. Stirring may be used during the mixing process to homogenize the contents of the round bottom flask.
[0024] In a nitrogen atmosphere, add 48-52wt% KOH aqueous solution to the first mixed liquid to react for 72-78 hours. Preferably, the rate of adding KOH aqueous solution should not be too fast so that the reactants can fully contact and react. Specifically, after adding the KOH aqueous solution, the whole system was reacted in an ice-water bath for 2-4 hours, and then transferred to 20-25° C. to continue the reaction for 70-74 hours to obtain the second mixed solution.
[0025] Add ice water and an acid for adjusting the pH of the second mixed solution to 1-2 to th...
Embodiment 1
[0049] (1) Add 10 mL of anhydrous DMF to a 200 mL round-bottomed flask, stir and add 1.5 g of NaH in an ice-water bath to obtain the third mixed solution. Dissolve 1g of 2,6-dihydroxyacetophenone in 20mL of anhydrous DMF, and slowly add the above third mixed solution within 30min in a nitrogen atmosphere; then dissolve 4mL of chloromethyl methyl ether in 5mL of anhydrous DMF, Continue to slowly add the above reaction mixture. Then, the reaction was stirred at 20°C for 6 h, 100 mL of ice water was added, extracted three times with 450 mL of ethyl acetate, the organic layers were combined, and washed with anhydrous Na 2 SO 4 After drying, the solvent was removed under reduced pressure to obtain 1.4 g of crude 2,6-dimethoxymethoxyacetophenone.
[0050] (2) Add 0.5g of 3,4,5-trihydroxybenzaldehyde, 4.5g of anhydrous K to a 500mL round bottom flask 2 CO 3 and 100mL of acetone, placed in an ice-water bath and stirred to obtain the fourth mixed solution. In a nitrogen atmosphere...
Embodiment 2
[0056] (1) Add 20 mL of anhydrous DMF to a 500 mL round bottom flask, stir and add 4 g of NaH in an ice-water bath to obtain the third mixed solution. Dissolve 2g of 2,6-dihydroxyacetophenone in 40mL of anhydrous DMF, and slowly add the above-mentioned third mixed solution within 30min in a nitrogen atmosphere; then dissolve 12mL of chloromethyl methyl ether in 20mL of anhydrous DMF, and continue to slowly Add the above reaction mixture. Then, the reaction was stirred at 25°C for 5 h, 200 mL of ice water was added, extracted three times with 800 mL of ethyl acetate, the organic layers were combined, and washed with anhydrous Na 2 SO 4 After drying, the solvent was removed under reduced pressure to obtain 3 g of crude 2,6-dimethoxymethoxyacetophenone.
[0057] (2) Add 1g of 3,4,5-trihydroxybenzaldehyde, 8g of anhydrous K to a 500mL round bottom flask successively 2 CO 3 and 100mL of acetone, placed in an ice-water bath and stirred to obtain the fourth mixed solution. In a ...
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