Preparation method of antibacterial drug
A technology for antibacterial drugs and compounds, applied in the field of preparation of antibacterial drugs, can solve the problems of limited extraction yield, limited practical application of compounds and the like
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[0024] Such as figure 1 Shown, the preparation method of the antibacterial drug of one embodiment, comprises the steps:
[0025] Step S110: under the condition of anhydrous and 50°C-80°C, sodium methoxide, the structural formula is Compound A and iodomethane react in alcohol to obtain the structural formula Compound B.
[0026] Wherein, the molar ratio of sodium methoxide to compound A is 5-12:1; the molar ratio of methyl iodide to compound A is 7-16:1.
[0027] Specifically, under the condition of anhydrous and 50°C-80°C, the step of reacting sodium methoxide, compound A and methyl iodide in alcohol is specifically: under the condition of anhydrous and 0°C-40°C, compound A Dissolve in alcohol to obtain the alcohol solution of Compound A, then add sodium methoxide to the alcohol solution of Compound A, and add methyl iodide at -10°C to 5°C, and then react at 50°C to 80°C for 6 hours to 15 hours, then quench the reaction. Wherein, the reagent used in the quenching reacti...
Embodiment 1
[0055] The preparation process of the antibacterial drug of the present embodiment is as follows:
[0056] (1) Dissolve compound A (102mmol) in 240 ml of anhydrous methanol to obtain a methanol solution of compound A; at 25°C, add anhydrous sodium methoxide powder (816mmol) to the methanol solution of compound A, stir and mix Cool down to 0°C after 0.5 hours, then add iodomethane (1430mmol), stir and mix for 0.5 hours, then heat up to 64°C, react at 64°C for 8 hours, cool to 25°C, then quench the reaction with 2mol / L hydrochloric acid to obtain The reaction solution was extracted with ethyl acetate, the organic phase was washed with a saturated aqueous solution of sodium sulfite, then dried with anhydrous sodium sulfate, filtered to remove sodium sulfate, the organic phase was concentrated in vacuo, and finally the concentrated organic phase was purified by silica gel column chromatography to obtain 23.1g of compound B, yield 90%, wherein, the detection data of compound B are ...
Embodiment 2
[0089] The preparation process of the antibacterial drug of the present embodiment is as follows:
[0090] (1) Dissolve compound A (102mmol) in 200 ml of absolute ethanol to obtain an ethanol solution of compound A; at 35°C, add anhydrous sodium methoxide powder (1224mmol) to the ethanol solution of compound A, stir and mix Cool down to -10°C after 0.5 hours, then add iodomethane (1632mmol), stir and mix for 0.5 hours, then heat up to 78°C, and react at 78°C for 12 hours, cool to 35°C, then quench the reaction with 2mol / L hydrochloric acid, The resulting reaction solution was extracted with ethyl acetate, the organic phase was washed with a saturated aqueous solution of sodium sulfite, then dried over anhydrous sodium sulfate, filtered to remove sodium sulfate, the organic phase was concentrated in vacuo, and finally the concentrated organic phase was purified by silica gel column chromatography. Obtain 12.8g of compound B, yield 50%, wherein, the detection data of compound B ...
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