Preparation method of cefazolin sodium with previous research quality and medicine preparation of cefazolin sodium
A technology for cefazolin sodium and preparation, which is applied in the field of preparation of the original development quality cefazolin sodium, can solve the problems of cefazolin sodium solvent residue and high water content, high production cost, reduced production efficiency, etc. The effect of using freeze-drying technology to control solvent residues and improve production efficiency
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[0021] Example 1 (Preparation of Cefazolinic Acid)
[0022] Add 500g of boron trifluoride-dimethyl carbonate solution to 500g of dimethyl carbonate, add 150g of 2-mercapto-5-methyl-1,3,4-thiadiazole and 300g of 7-ACA while stirring and increase the temperature to 35~40℃ After the reaction, add 500ml of dimethylformamide, stir for 10 minutes, slowly add hydrochloric acid within 20 minutes to a pH of 2 to 3, adjust the temperature to 25-35 ℃, react for 60 minutes, filter, and wash with acetone twice , Dried in vacuum to obtain crude TDA;
[0023] Dichloromethane, tetrazolium acetic acid, triethylamine, pivaloyl chloride to prepare mixed acid anhydride;
[0024] Add crude TDA to dichloromethane solvent, lower the temperature to -30℃, add tetramethylguanidine dropwise within 30 minutes, and then add dropwise mixed acid anhydride to control the temperature. After phase separation, extraction, crystallization and other steps, cefazolinic acid is prepared The crystals are then purified an...
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[0025] Example 2 (Preparation of Cefazolin Sodium)
[0026] Put 45.5kg of cefazolinic acid and 280kg of acetonitrile into a 1000L enamel kettle at room temperature, stir, add 82kg of 5% sodium hydroxide aqueous solution to adjust PH≈7, start to cool to -5~-10℃, stand for layering, acetonitrile Add 15 kg of anhydrous sodium sulfate to the layer and dry for 2 hours. Check that the moisture content of the mother liquor of acetonitrile is 1.4%. Filter out the sodium sulfate, and then filter the mother liquor with a precision filter. The mother liquor is distilled under reduced pressure at 25~30℃ with a high vacuum multistage Roots pump. When the temperature is between -0.09MPa~-0.1MPa, when the solid is precipitated out, stop the distillation, reduce the temperature to 0~5℃, stir for 2h, centrifuge, the filter cake is vacuum dried with high vacuum multi-stage Roots pump, and the temperature is 30~ 40℃, vacuum degree -0.09MPa~-0.1MPa, after drying, 43.6kg of cefazolin sodium was obtai...
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[0027] Example 3 (Preparation of Cefazolin Sodium)
[0028] Put 45.5kg of cefazolinic acid and 280kg of acetonitrile into a 1000L enamel kettle at room temperature, stir, add 41kg of 10% sodium hydroxide aqueous solution to adjust PH≈7, start to cool to -5~-10℃, stand for layering, acetonitrile Add 15 kg of anhydrous sodium sulfate to the layer and dry for 2 hours. Check that the moisture content of the mother liquor of acetonitrile is 1.6%, filter out the sodium sulfate, and then filter the mother liquor with a precision filter. The mother liquor is distilled under reduced pressure at 20~25℃ with a high vacuum multistage Roots pump. When the temperature is between -0.09MPa~-0.1MPa, when the solid is precipitated out, stop the distillation, reduce the temperature to 0~5℃, stir for 2h, centrifuge, the filter cake is vacuum dried with high vacuum multi-stage Roots pump, and the temperature is 30~ 40℃, vacuum degree -0.09MPa~-0.1MPa, after drying, 43.0kg of cefazolin sodium was obta...
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