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With hydrogenchloride; In ethanol; for 2h;Reflux; Green chemistry; |
20g of leucovorin and 70ml of water were put into the reaction flask, heated to 110 C with stirring, and 33ml of N-methylpiperazine was added dropwise. After half an hour dripping finished, the mixture was incubated for 10 hours, sampled and analyzed, and transformed into 94%. The mixture was cooled to 70-80 C and then distilled under reduced pressure to recover water and methylpiperazine. After steaming, 200 ml of ethanol was added and 15 ml of hydrochloric acid was added under stirring to reflux for 2 hours. The mixture was cooled to room temperature and filtered to obtain 56 g of tide (incomplete pumping Dry), do not dry direct secondary beating, add water, 9% ethanol 165ml heat reflux 1h. Cooling filtration, too tidal goods 28.14g, do not dry directly to the third beating, adding 95% ethanol 180ml, heated to reflux1h, cooled and filtered, washed with a small amount of anhydrous ethanol, dried, to obtain 19.86g liquid phase content of 99.43% <strong>[100986-85-4]levofloxacin</strong> hydrochlorideProducts, like white solid. Beating mother liquor was concentrated and recovered to obtain 4.13g of crude product, the content of 93.3%. Total yield of 86%, of which finished products receivedRate of 72.7%. Products can be further recovered from the secondary mother liquor, the cumulative yield of up to 90% |
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With hydrogenchloride; In ethanol; water; for 8h;Reflux; |
20g left oxycyclic acid, 70ml water into the reaction flask, heated to 120 C with stirring,38 ml of N-methylpiperazine are initially added dropwise,End half an hour, insulation 15 hours, sampling analysis, conversion 95%. After cooling to 70-80 C and distillation under reduced pressure,Recovering water and methylpiperazine, steaming and adding 200 ml of ethanol, adding 15 ml of hydrochloric acid while stirring, heating and refluxing for 2 hours, cooling to room temperature, filtering to obtain tide product 60g (not completely drained), not directly drying and performing secondary beating , Adding 165ml of 9% aqueous ethanol and heating to reflux for 3h. Cooled and filtered to obtain tide product 29.02g, do not directly dry the third beating, add 95% ethanol 180ml, heated to reflux 3h, cooled and filtered, a small amount of ethanol washing and drying, to obtain 21.03g liquid content of 99.56% <strong>[100986-85-4]Levofloxacin</strong> hydrochloride finished product, white-like solid. Beating mother liquor was concentrated and recovered, to obtain 4.34g crude, content of 92.8%. The total yield of 88%, of which yield of 72.7%. Products can be further recovered from the secondary mother liquor, the cumulative yield of up to 90% |
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With hydrogenchloride; In ethanol; water; for 2h;Reflux; |
20g of L-Oxalaconic acid,70ml water is put into the reaction bottle,Heat to 110C with stirring33 ml of N-methylpiperazine was added dropwise.After half an hour drip, keep warm for 10 hours.Sampling analysis, conversion 94%.After cooling to 70-80 deg.] C under reduced pressure by distillation,And recovering water-methylpiperazine,200ml of ethanol was added after steaming.15ml of hydrochloric acid was added under stirring.Heat reflux 2h,Cool to room temperature, filter,56g (not completely drained)Direct drying without drying165 ml of 9% aqueous ethanol was added and the mixture was heated at reflux for 1 h.Cooled and filtered, the product was 28.14g.Do not dry directly for the third time,Add 95% ethanol 180ml, heated to reflux for 1h,Cooling filtration, a small amount of anhydrous ethanol washing,After drying, 19.86 g of finished <strong>[100986-85-4]levofloxacin</strong> hydrochloride with a liquid phase content of 99.43% was obtained.White solid.Beating mother liquor is concentrated and recovered.4.13 g of crude product are obtained with a content of 93.3%.Total yield 86%Wherein product yield 72.7%. The product can be further recovered from the secondary mother liquor,The cumulative yield of 90%. |
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