Method for synthesizing high-purity gamithromycin
A technology of gamimycin and its synthesis method, which is applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of difficult industrialization and low product purity, and achieve easy industrial production and simple synthesis process , easily accessible effects
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Embodiment 1
[0036] Configuration transformation (synthesis of Z-erythromycin oxime):
[0037] Take thiocyanate E-erythromycin oxime hydrochloride (105.2g, 68.76mmol, content 55.20%) and place it in a 2L reaction flask, add 840mL of distilled water, after adding, stir for 10min to obtain a suspension; h 2 O (10.0g, 238mmol) was dissolved in 210mL of water, and the resulting solution was added to the suspension. After the addition was complete, under the protection of nitrogen, the mixture was stirred at room temperature for 16 hours. After the reaction was monitored by TLC, it was followed by post-processing.
[0038] Post-treatment: After the reaction solution becomes clear, filter, add ethyl acetate twice for extraction (350mL for the first time, 150mL for the second time), combine the organic layers, wash once with 150mL saturated sodium chloride brine, and add 450mL of Dichloromethane, stirred evenly, crystals precipitated out soon, cooled to -5°C to 0°C, stirred for 4h, filtered, and...
Embodiment 2
[0050] Configuration conversion:
[0051] Take thiocyanate E-erythromycin oxime hydrochloride (105.2g, 68.76mmol, content 55.20%) and place it in a 2L reaction flask, add 630mL of distilled water, after adding, stir for 10min to obtain a suspension; h 2 O (2.89g, 68.76mmol) was dissolved in 105mL water, and the resulting solution was added to the suspension. After the addition was complete, under the protection of nitrogen, the mixture was stirred at room temperature for 8 hours. After the reaction was monitored by TLC, it was followed by post-processing.
[0052] Post-treatment: After the reaction solution becomes clear, filter, add ethyl acetate twice for extraction (315mL for the first time, 105mL for the second time), combine the organic layers, wash once with 150mL saturated sodium chloride brine, and add 315mL of Dichloromethane, stirred evenly, crystals precipitated out soon, cooled to -5°C to 0°C, stirred for 2h, filtered, and dried at room temperature to obtain 41.97...
Embodiment 3
[0064] Configuration conversion:
[0065] Take thiocyanate E-erythromycin oxime hydrochloride (105.2g, 68.76mmol, content 55.20%) and place it in a 2L reaction flask, add 1260mL of distilled water, after adding, stir for 10min to obtain a suspension; h 2 O (14.44g, 68.76mmol) was dissolved in 420mL of water, and the resulting solution was added to the suspension. After the addition was complete, under the protection of nitrogen, stirred at room temperature for 20h. After the reaction was monitored by TLC, it was followed by post-processing.
[0066] Post-processing: After the reaction solution becomes clear, filter, add ethyl acetate twice for extraction (630 mL for the first time, 210 mL for the second time), combine the organic layers, wash once with 200 mL saturated sodium chloride brine, and add 630 mL of Dichloromethane, stirred evenly, crystals precipitated out soon, cooled to -5°C to 0°C, stirred for 6h, filtered, and dried at room temperature to obtain 46.84g of Z-ery...
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