Synthetic method of antibiotic cefixime
A technology of cefixime and synthetic method, applied in the direction of antibacterial drugs, organic chemistry, etc., can solve problems such as unfavorable continuity, large-scale industrial production, expensive tetrahydrofuran, harsh reaction conditions, etc., to shorten the production cycle and simplify Effects on manipulation, yield enhancement and purity
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[0015] Example 1
[0016] In a 1000L reactor, add 500L of acetone, 50kg of AVCA, 75kg of MICA-active ester, 50L of methanol, add 25kg of triethylamine dropwise at 5°C for about 1.5h (hours), and keep the reaction at 5°C for 4h (hours). Take a sample (the intermediate is less than 0.3%).
[0017] After the reaction is over, acetone and methanol are recovered under reduced pressure at 40°C. The recovered acetone and methanol can be used directly. After steaming, 400L purified water is added, 400L ethyl acetate is cooled to 10°C, and the mixture is separated for 30 minutes and collected. The water phase, the water phase was extracted twice with 200L ethyl acetate, the water phase was collected and filtered to remove insoluble materials.
[0018] Add 8 kg of activated carbon to the water phase, stir for 30 min, filter, and then wash the filter cake with 200 L of purified water, and combine the filtrate and washing liquid.
[0019] Add 200L of acetone to the water phase and lower the t...
Example Embodiment
[0021] Example 2
[0022] In a 1000L reactor, add 500L of acetone, 50kg of AVCA, 90kg of MICA-active ester, 50L of purified water, add 25kg of triethylamine dropwise at 10 degrees for about 2.5 hours, keep the reaction at 5 degrees for 4 hours, and sample (the intermediate is less than 0.3 %).
[0023] After the reaction, the acetone is recovered by distillation under reduced pressure at 45°C. The recovered ketone can be used directly. After steaming, add 500L of purified water and 400L of ethyl acetate to cool to 10°C. Separate for 30 minutes at rest. Collect the water phase and water. The phase was extracted twice with 200L ethyl acetate, the aqueous phase was collected and filtered to remove insoluble materials.
[0024] Add 3 kg of activated carbon to the water phase, stir for 30 min, filter, and then wash the filter cake with 200 L of purified water, and combine the filtrate and washing liquid.
[0025] Add 200L of acetone to the water phase and lower the temperature to below...
Example Embodiment
[0027] Example 3,
[0028] Mix 7-AVCA and MICA active ester with a weight ratio of 1:1.5 and place them in a mixed solvent with a volume ratio of acetone and methanol of 1:30 and a volume ratio of purified water to water of 1:30. Sodium hydroxide or Potassium hydroxide was adjusted to pH 7.0, dissolved and acylated at a temperature of -20℃ to obtain cefixime intermediate A solution; the obtained cefixime intermediate A solution was extracted with ethyl acetate solvent, and then In the obtained water phase, 0.1% of the 7-AVCA feed amount of activated carbon was added to the water phase for decolorization, and then 0.1% of the 7-AVCA feed amount of EDTA was added to obtain an aqueous solution of cefixime intermediate A; The weight ratio is 1:1,
[0029] When the acylation reaction is over, set the vacuum distillation to recover acetone and methanol at 40°C. The recovered acetone and methanol can be used directly. After steaming, add 3 times the amount of 7-AVCA pure water, and 7-AVC...
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