Roxithromycin impurity J and preparation method thereof
A technology of roxithromycin and erythromycin, which is applied in the field of roxithromycin impurity J and its preparation, can solve the problems of fewer impurity preparation process reports, etc., so as to improve the quality of roxithromycin finished products, strengthen control, Improve the effect of accurate positioning and qualitative
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[0026] The preparation method of roxithromycin impurity J comprises dissolving the oximation product of erythromycin A and its salt in a solvent, adding an acid-binding agent, and under the action of the acid-binding agent, adding 2-chloro Carry out the synthesis reaction of ethoxychloromethane for 1-24 hours, evaporate the reaction solvent to dryness, add lower alcohol or lower ketone to dissolve and refine, filter, drop water to crystallize, filter and dry to obtain roxithromycin impurity J.
[0027] The concrete addition amount of each material is as follows, by mass ratio:
[0028] The oximation product of erythromycin A and its salt 1; 2-chloroethoxychloromethane 0.2~0.3; acid binding agent 0.3~0.4; synthetic solvent 2~3; refining solvent 2~3; water 3~5. The preparation method of Roxithromycin impurity J according to claim 2, is characterized in that: described synthesis solvent is methylene chloride, chloroform, ethyl acetate or DMF.
[0029] The lower alcohol in the re...
specific Embodiment 1
[0033] In a 100ml reaction bottle, add 10g of erythromycin A oxime and 50ml of dichloromethane, stir to dissolve, add 6ml of 30% sodium hydroxide solution, and add 3.3g of 2-chloroethoxychloromethane dropwise at a temperature below 10°C , keep the reaction for more than 2 hours, the reaction is over, concentrate to dryness at 60°C, dissolve the residue with 40ml of acetone, filter, control the temperature at 30-35°C, slowly add 100ml of water dropwise, until the solid precipitates, after 1 hour of heat preservation, it drops to Suction filtration at 20°C, and the filter cake was vacuum-dried at 55°C to obtain 7.5 g of a white solid. Yield 75%, content 98.5%.
specific Embodiment 2
[0034] In a 100ml reaction bottle, add 10g of erythromycin A oxime and 50ml of chloroform, stir to dissolve, add 6ml of 30% sodium hydroxide solution, add 3.3g of 2-chloroethoxychloromethane dropwise below 10°C, and react After 2 hours, the reaction was completed, concentrated to dryness at 70°C, the residue was dissolved in 40ml of methanol, filtered, and the temperature was controlled at 30-35°C, and 100ml of water was slowly added dropwise until the solid precipitated. Vacuum drying at 55°C yielded 7.8 g of a white solid. Yield 78%, content 98.3%.
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