Synthesis process of erythromycin oxime
A technology of erythromycin oxime and a synthesis method, which is applied in the synthesis field of erythromycin oxime, can solve the problems of high temperature and pH control requirements, complicated processes and the like, and achieves the effects of simple operation, safe and reliable operation
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Embodiment 1
[0008] Heat 100L of erythromycin fermented pre-extracted solution, that is, mixed butyl acetate extract, to 30°C in a reaction kettle, add 2% of the total volume of saturated saline, stir for 0.5-1 hour, and let it stand for more than 2 hours , to remove the lower layer of water and impurities. The mixed butyl acetate extract of the above-mentioned purified erythromycin is warmed up to 40°C, and is added in a stirring state by the weight ratio of hydroxylamine hydrochloride: triethylamine=1.5:1. The purpose of this operation is to control the reaction solution at pH = 5.5, stir at 30°C for 16-24 hours, monitor the reaction with a common thin-layer chromatography method, separate the reaction liquid from solid to liquid, and the solid is erythromycin oxime hydrochloride. Then the solid erythromycin oxime hydrochloride of gained is dropped in the reaction kettle by the weight ratio of solid erythromycin oxime hydrochloride: methyl alcohol=1: 1.5, keep temperature 10 ℃, adjust so...
Embodiment 2
[0010] Heat 100L erythromycin fermented pre-extracted liquid, that is, mixed butyl acetate extract, to 40°C in a reaction kettle, add saturated saline water accounting for 4% of the total volume, stir for 0.5-1 hour, and let it stand for more than 2 hours , to remove the lower layer of water and impurities. The mixed butyl acetate extract of the above-mentioned purified erythromycin is warmed up to 55°C, and is added in a stirring state by the weight ratio of hydroxylamine hydrochloride: triethylamine=2:1. The purpose of this operation is to control the reaction solution at pH = 6, stirred at 60°C for 16-24 hours, and after the reaction was monitored by common thin-layer chromatography, the reaction liquid was separated from solid to liquid, and the solid was erythromycin oxime hydrochloride. Then the solid erythromycin oxime hydrochloride of gained is dropped in the reaction kettle by the weight ratio of solid erythromycin oxime hydrochloride: methyl alcohol=1: 2, keep temper...
Embodiment 3
[0012] Heat 100L erythromycin fermented pre-extracted liquid, that is, mixed butyl acetate extract, to 50°C in a reaction kettle, add 5% of the total volume of saturated saline, stir for 0.5-1 hour, and let it stand for more than 2 hours , to remove the lower layer of water and impurities. The mixed butyl acetate extract of the above-mentioned purified erythromycin is warmed up to 70°C, and is added in a stirring state by the weight ratio of hydroxylamine hydrochloride: triethylamine=2.5:1. The purpose of this operation is to control the reaction solution at pH = 7, stirred at 70°C for 16-24 hours, and after the reaction was monitored by common thin-layer chromatography, the reaction liquid was separated from solid to liquid, and the solid was erythromycin oxime hydrochloride. Then the solid erythromycin oxime hydrochloride of gained is dropped in the reaction kettle by the weight ratio of solid erythromycin oxime hydrochloride: methyl alcohol=1:3, keep temperature 30 ℃, adjus...
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