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Novel ampicillin sodium compound
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A technology of ampicillin sodium and compound, applied in the field of medicine, can solve problems such as inconvenience in clinical use
Inactive Publication Date: 2016-08-24
石药集团中诺药业(石家庄)有限公司
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This brings a lot of inconvenience to clinical use
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Embodiment 1
[0032] Embodiment 1 prepares new ampicillin sodium compound of the present invention
[0033] Add 100 g of ampicillin sodium crude product into a 15 L three-necked flask, add 6000 mL of isobutanol and 200 mL of N-methylpyrrolidone, stir and heat to reflux to dissolve, then add 800 mL of ether to the solution, then slowly cool down to 10 °C, stir and analyze crystallized, filtered, washed with ether, and dried under vacuum at 65°C to obtain 956 g of the new ampicillin sodium compound with a yield of 95.6%.
[0034] The X-raypowder diffraction pattern of the new ampicillin sodium compound prepared in embodiment 1 is (accuracy is ± 0.1 °): 4.95 °, 6.38 °, 10.11 °, 11.53 °, 12.63 °, 12.82 °, 13.91 ° at reflection angle 2θ °, 14.17°, 14.56°, 14.87°, 15.08°, 15.57°, 16.26°, 16.60°, 18.73°, 18.93°, 19.29°, 19.93°, 20.28°, 20.73°, 20.98°, 21.23°, 21.92°, Features at 22.56°, 22.81°, 23.01°, 23.80°, 24.14°, 24.47°, 25.43°, 25.63°, 26.08°, 26.33°, 26.74°, 27.07°, 27.78°, 28.43°, 29.0...
Embodiment 2
[0036] Embodiment 2 prepares new ampicillin sodium compound of the present invention
[0037] Add 100g of ampicillin sodium crude product into a 15L three-necked flask, add 8000mL of isobutanol and 100mL of N-methylpyrrolidone, stir and heat to reflux to dissolve, then add 1000mL of ether to the solution, then slowly cool down to 15°C, stir and analyze crystallized, filtered, washed with ether, and dried under vacuum at 55°C to obtain 913g of the new ampicillin sodium compound with a yield of 91.3%.
[0038] The X-raypowder diffraction pattern and the DSC collection of illustrative plates of the new ampicillin sodium compound prepared in embodiment 2 are the same as in embodiment 1.
Embodiment 3
[0039] Embodiment 3 prepares new ampicillin sodium compound of the present invention
[0040] Add 100 g of ampicillin sodium crude product into a 15 L three-necked flask, add 5000 mL of isobutanol and 240 mL of N-methylpyrrolidone, stir and heat to reflux to dissolve, then add 600 mL of ether to the solution, then slowly cool down to 5 °C, stir and analyze crystallized, filtered, washed with ether, and dried under vacuum at 75°C to obtain 928g of the new ampicillin sodium compound with a yield of 92.8%.
[0041] The X-ray powder diffraction pattern and the DSC collection of illustrative plates of the new ampicillin sodium compound prepared in embodiment 3 are the same as in embodiment 1.
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Abstract
The invention relates to a novel ampicillinsodium compound and a preparation method thereof and belongs to the technical field of medicine. According to the ampicillinsodium compound, in an X-raypowderdiffraction spectrum obtained through Cu-Ka radionetric measurement, characteristic peaks are displayed at the positions where 2theta equals to 14.17 + / -0.1 degrees, 14.56 + / -0.1 degrees, 14.87 + / -0.1 degrees and 26.74 + / -0.1 degrees. The prepared novel ampicillinsodium compound is good in mobility, more meets requirements of technology of pharmaceutics and is more suitable for preparing various pharmaceutic preparations. Due to the fact that powder-injection prepared from the novel ampicillin sodium compound is good in stability, besides, stability can reach 36 hours or above after the powder-injection is prepared into an injection solution, storage time is greatly prolonged, therefore safety and efficiency of drug use are improved, and the occurrence rate of adverse reactions is reduced.
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