Crystal of penicillin derivant and preparation method thereof
A technology of crystal, fururonil penicillin, which is applied in the field of preparation of broad-spectrum semi-synthetic penicillin, can solve the problems that impurities cannot be effectively removed, and achieve the effects of convenient transportation and storage, good industrial applicability, and stable crystal properties
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Embodiment 1
[0021] Refer to the synthesis method of USP 3959258 to prepare 300 mL of 0.148 mol / L fururacillin penicillin acid ethyl acetate solution, cool in an ice-salt bath at 0°C, add 200 mL of 0.5 mol / L sodium bicarbonate solution dropwise, adjust the pH to about 7.5, and stir 10min, stand still for phase separation, move the water phase into a reaction flask, add 200mL ethyl acetate, dropwise add 3N hydrochloric acid to pH=2 below 0°C, stir for 10min, stand still for phase separation; extract the water phase once with 50mL ethyl acetate, The organic phases were combined and dried by adding anhydrous magnesium sulfate. Filtrate, evaporate about 2 / 3 of the volume of ethyl acetate under reduced pressure, let stand for crystallization, wait for a large amount of crystals to precipitate, cool and filter, wash with pulp, filter and dry, and vacuum dry to obtain the product with a yield of 70.7%.
[0022] Use D / max-IIIA DIFFRATOMETER (RIGAKU CORPORATION, JANPAN) X-diffraction instrument, wi...
Embodiment 2
[0027] The reaction product prepared according to the synthesis method of Example 1 is 300 mL of 0.137 mol / L fururobenzyl penicillin acid dichloromethane solution, cooled in an ice-salt bath to 0° C., and 200 mL of 0.5 mol / L sodium bicarbonate solution was added dropwise to adjust the pH= 7 or so, stir for 10 minutes, stand still for phase separation, move the water phase into a reaction flask, add 200 mL of dichloromethane, add 2N sulfuric acid dropwise below 0°C until PH = 2, stir for 10 min, stand still for phase separation; use 50 mL of dichloromethane for the water phase Extracted once with methane, combined the organic phases, added anhydrous magnesium sulfate and dried. Filtrate, evaporate a large amount of dichloromethane under reduced pressure to form a supersaturated solution, stand for crystallization, wait for a large amount of crystals to precipitate, cool and filter, wash with pulp, filter and dry, and vacuum dry to obtain the product with a yield of 73.9%. Measu...
Embodiment 3
[0029] According to the synthetic method of ("Chinese Journal of Medicinal Chemistry" 2006, 2, 16 (1), 51), 300 mL of 0.137 mol / L fururobenzyl penicillin acid trichloromethane solution was prepared, cooled in an ice-salt bath to 0 ° C, and slowly added dropwise 0.5 200mL of mol / L sodium hydroxide solution, adjust the pH to about 8, control the temperature, then add 200mL of ice water, stir for 10min, let stand to separate the phases, transfer the water phase into the reaction bottle, add 200mL of chloroform, and cool in an ice-salt bath To below 0°C, slowly add 2N phosphoric acid dropwise to PH = 2.5, stir for 10 minutes, stand still and separate the phases; extract the aqueous phase once with 50 mL of chloroform, combine the organic phases, and add anhydrous magnesium sulfate to dry. Filtrate, evaporate a large amount of dichloromethane under reduced pressure to form a supersaturated solution, let stand to crystallize, wait for a large amount of crystals to precipitate, cool a...
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