Synthetic method of furbenicillin acid
A technology of furbenicillin acid and a synthetic method, which is applied in the field of synthesis of semi-synthetic antibiotics, can solve problems such as environmental pollution, complicated processes, large toxic and side effects, and achieves shortening of technological operation procedures, superior quality and cost, and improved product quality. Effect
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Embodiment 1
[0030] Add 210kg of dichloroethane and 16.5kg of 6-APA into the dry reaction tank, add 27kg of triethylamine and stir to dissolve, dissolve in about 1.5 hours, cool down to 0°C, and press into the high level tank for later use.
[0031] Add 320kg ethylene dichloride and 21kg sodium furylureidophenylacetate in another dry reaction tank, add 0.09kg N-methylmorpholine and 7.3kg ethyl chloroformate sequentially at room temperature, and react under stirring After 1.5 hours, cool down to -10°C, add dropwise to the 6-APA amine salt solution in the high-level tank, and keep it at -5~0°C for 1 hour to react.
[0032] The reaction liquid was warmed up to room temperature, alkalized with 5% aqueous sodium hydroxide solution until the pH of the solution was 5.5-6.7, and left to stand to separate the phases of the solution and recover the organic phase. Add 120L ethyl acetate to the water phase, add 9% dilute hydrochloric acid dropwise, acidify to pH=2-3, let stand to separate the layers, ...
Embodiment 2
[0034] Add 180kg of chloroform and 16kg of 6-APA into a dry reaction tank, add 27kg of diisopropylamine and stir to dissolve, dissolve in about 1.5 hours, cool down to 0°C, and press into a high-level tank for later use.
[0035] Add 370kg chloroform and 21kg sodium furylureidophenylacetate in another dry reaction tank, add 0.11kg N-ethylmorpholine and 7.5kg ethyl chloroformate sequentially at room temperature, react 1.5kg under stirring h, lower the temperature to -10°C, add dropwise to the 6-APA amine salt solution in the high-level tank, and keep it at -5-0°C for 1 hour to react after dropping.
[0036] The reaction solution was warmed up to room temperature, basified with 8% sodium carbonate aqueous solution until the pH of the solution was 5.5-6.7, and allowed to stand still to separate the phases of the solution and recover the organic phase. Add 120L of ethyl acetate to the water phase, add dropwise 6% phosphoric acid to acidify to pH=2-3, let stand to separate the laye...
Embodiment 3
[0038] Add 200kg of trichloroethane and 16kg of 6-APA into a dry reaction tank, add 20kg of diethylamine and stir to dissolve, dissolve in about 1.5 hours, cool down to 0°C, and press into a high-level tank for later use.
[0039] In another dry reaction tank, add 310kg trichloroethane and 21kg sodium α-furylureidophenylacetate, add 0.18kg N-ethylmorpholine and 7.8kg ethyl chloroformate sequentially at room temperature, and react under stirring After 1.5 hours, cool down to -10°C, add dropwise to the 6-APA amine salt solution in the high-level tank, and keep it at -5~0°C for 1 hour to react.
[0040]The reaction solution was warmed up to room temperature, basified with 10% aqueous sodium bicarbonate solution until the pH of the solution was 5.5-6.7, and allowed to stand still to separate the phases of the solution and recover the organic phase. Add 180L of chloroform to the water phase, add 3% sulfuric acid dropwise to acidify to pH=2-3, let stand to separate the layers, and d...
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