Refining method of valnemulin hydrochloride
A technology of vonimulin hydrochloride and purification method, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of sulfides, etc., can solve the problems of high equipment cost, physical injury of operators, difficulty in solvent recovery, etc. The use of expensive equipment, the reduction of production costs, and the effect of obvious purification effects
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Embodiment 1
[0021] Take 500ml of the methyl tert-butyl ether solution of warnimulin base with a mass-volume concentration of 5%, add purified water (i.e. 250ml purified water) 0.5 times the volume of the above solution, heat to 40°C, stir for 0.5h, and let it stand Separate the layers, take the upper organic phase, and discard the lower aqueous phase. Add 600 ml of ethanol solution with a mass volume concentration of 10% to the organic phase, stir at room temperature for 0.5 h, let stand to separate layers, take the upper organic phase, and discard the lower aqueous phase. Pass dry hydrogen chloride gas into the organic layer obtained above, stir slowly at room temperature for 2 hours, a large number of crystals are precipitated, and slowly cool down to 0 °C at a rate of 5 °C per hour, the crystallization is complete, and the precipitated product is filtered. Dry to obtain the solid product of warnemulin hydrochloride. Product yield: 99%. Purity: 99.8%. Moisture: 1.2%. Total impurity:...
Embodiment 2
[0023] Take 500ml of the methyl tert-butyl ether solution of warnemulin base with a mass-volume concentration of 6%, add 300ml of purified water, heat to 40°C, stir for 1h, let stand to separate layers, take the upper organic phase, and discard the lower layer water box. Add 500 ml of ethanol solution with a mass volume concentration of 13% to the organic layer, stir at room temperature for 0.5 h, let stand to separate layers, take the upper organic phase, and discard the lower aqueous phase. Pass dry hydrogen chloride gas into the organic layer obtained above, stir slowly at room temperature for 3 hours, a large number of crystals are precipitated, and slowly lower the temperature to 0 °C at a rate of 4 °C per hour, the crystallization is complete, and the precipitated product is filtered. Dry to obtain the solid product of warnemulin hydrochloride. Product yield: 98%. Purity: 99.2%. Moisture: 1.5%. Total impurity: less than 0.8%.
Embodiment 3
[0025] Take 500ml of the methyl tert-butyl ether solution of warnimulin base with a mass-volume concentration of 7%, add 300ml of purified water, heat to 50°C, stir for 1h, let stand to separate layers, take the upper organic phase, and discard the lower layer water box. Add 700 ml of ethanol solution with a mass volume concentration of 15% to the organic layer, stir at room temperature for 1 h, let stand to separate layers, take the upper organic phase, and discard the lower aqueous phase. Pass dry hydrogen chloride gas into the organic layer obtained above, stir slowly at room temperature for 3 hours, a large number of crystals are precipitated, and slowly lower the temperature to 0 °C at a rate of 5 °C per hour, the crystallization is complete, and the precipitated product is filtered. Dry to obtain the solid product of warnemulin hydrochloride. Product yield: 98.8%. Purity: 98.9%. Moisture: 1.8%. Total impurity: less than 1%.
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