The method for crystallization production cefpiramide sodium crystal
A technology of cefpiramide sodium and cefpiramide acid, which is applied in the field of medicine and chemical industry, can solve the problems of easy precipitation, poor fluidity, poor solubility of amine salts, etc., and achieves the effects of good solubility, good fluidity and stable solution
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Embodiment 1
[0039]Accurately measure 20g of cefpiramin, 60ml of methanol, 40ml of acetone, 20ml of acetonitrile, and 4.6ml of triethylamine into a four-necked bottle. The molar ratio of cefpiramin and triethylamine is 1:1. The ratio of the weight in grams to the volume in milliliters of the solvent I is 1:6. In a constant temperature reaction bath at 20°C, stir until completely dissolved to form a cefpiramide salt solution for later use. Accurately measure 1.5g of sodium hydroxide and 40ml of methanol into a conical flask. The amount of sodium hydroxide added is such that the molar ratio of sodium hydroxide to cefpiramin is 1.15:1. Stir until completely dissolved to form a hydroxide Sodium solution for later use. In a constant temperature reaction bath at 20°C, the sodium hydroxide solution was evenly added to the cefpiramide salt solution within 20 minutes, and then 0.03 g of cefpiramide sodium crystals were added as seed crystals, and the crystals were grown for 10 minutes. Then add 30...
Embodiment 2
[0041] Accurately measure 20g of cefpiramin, 60ml of methanol, 40ml of acetone, 20ml of acetonitrile, and 4.6ml of diisopropylamine into a four-necked bottle. The molar ratio of cefpiramin and diisopropylamine is 1:1. The ratio of the weight in grams to the volume in milliliters of solvent I is 1:6. Stir in a constant temperature reaction bath at 10°C until it is completely dissolved to form a cefpiramide salt solution for later use. Accurately measure 5.42g of sodium isooctanoate and 150ml of acetone into a conical flask. The amount of sodium isooctanoate is to make the molar ratio of sodium isooctanoate to cefpiramide 1:1, and stir until completely dissolved to form sodium isooctanoate The solution is ready for use. In a constant temperature reaction bath at 25°C, the sodium isooctanoate solution was evenly added to the cefpiramide salt solution within 25 minutes, and then 0.02 g of cefpiramide sodium crystals were added as seed crystals, and the crystals were grown for 25 m...
Embodiment 3
[0043] Accurately measure 20g of cefpiramin, 60ml of methanol, 40ml of acetone, 10ml of water, and 4.6ml of diisopropylamine into a four-neck bottle. The molar ratio of cefpiramin and diisopropylamine is 1:1. The ratio of the weight in grams to the volume in milliliters of solvent I is 1:5.5. Stir in a constant temperature reaction bath at 20°C until it is completely dissolved to form a cefpiramide salt solution for later use. Accurately measure 5.42g of sodium isooctanoate and 150ml of acetone into a conical flask. The amount of sodium isooctanoate is to make the molar ratio of sodium isooctanoate to cefpiramide 1:1, and stir until completely dissolved to form sodium isooctanoate The solution is ready for use. In a constant temperature reaction bath at 15°C, the sodium isooctanoate solution was evenly added to the cefpiramide salt solution in 30 minutes, and then 0.04 g of cefpiramide sodium crystals were added as seed crystals, and the crystals were grown for 15 minutes. Th...
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