High-purity and/or high-content penicillin sodium salt solid powder and preparing method
A solid powder and solid technology, which is applied in the fields of active ingredients of heterocyclic compounds, anti-infective drugs, organic chemistry, etc. It can solve the problems of affecting product quality, easy decomposition, and many impurities in freeze-dried powder.
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Embodiment 1
[0026] Example 1 Preparation of ticarcillin disodium solid powder with content of 98.7% and purity of 99.68%
[0027] Add 2 mL of water to an ethyl acetate solution containing 0.02 mol of ticarcillin (formula I, Ar is thiophen-3-yl), add sodium bicarbonate at 5-10°C to adjust the pH to 6.5, and separate the water layer. The aqueous layer was slowly added dropwise to 100 mL of isopropanol, filtered with suction, washed the filter cake with a small amount of isopropanol, and vacuum-dried to obtain 7.9 g of ticarcillin disodium white powdery solid, with a yield of 93%. Purity 99.68% (HPLC), content 98.7%.
Embodiment 2
[0028] Example 2 Preparation of ticarcillin disodium solid powder with content of 98.5% and purity of 99.25%
[0029] Add 2 mL of water to the ethyl acetate solution containing 0.02 mol of ticarcillin, add sodium carbonate at 5-10°C to adjust the pH to 6.5, and separate the water layer. The water layer was slowly added dropwise to 100 mL of tert-butanol, filtered with suction, washed the filter cake with a small amount of tert-butanol, and vacuum-dried to obtain ticarcillin disodium as a white powdery solid with a purity of 99.25% and a content of 98.5%.
Embodiment 3
[0030] Example 3 Preparation of ticarcillin disodium solid powder with content of 99.0% and purity of 99.82%
[0031] Add 2 mL of water to the ether solution containing 0.02 mol of ticarcillin, add sodium bicarbonate at 5-10°C to adjust the pH to 6.5, and separate the water layer. The aqueous layer was slowly added dropwise to 500 mL of acetone, filtered with suction, washed with a small amount of acetone, and dried in vacuum to obtain ticarcillin disodium as a white powdery solid with a purity of 99.82% and a content of 99.0%.
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