Purification method for protective meropenem
A technology of meropenem and purification method, which is applied in the field of medicinal chemical synthesis, can solve the problems such as inability to effectively remove impurities, and achieve the effects of reducing content, good purification effect and simple operation
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Embodiment 1
[0051] A purification method for protecting meropenem, comprising the following steps:
[0052] (1) Add 99.54g of N,N-dimethylformamide and 15g of meropenem side chains to the reaction flask, stir and dissolve to obtain a clear solution, add 25g of meropenem core to it, stir the solution until it becomes clear, and cool down to
[0053] -60~-50℃, gradually drop 7.42g N,N-diisopropylethylamine into the reaction bottle
[0054] , and reacted for 18 hours to obtain a protected meropenem feed solution.
[0055] The content of impurity IV in the side chain of meropenem was 6ppm, and the content of impurity V in the protected meropenem feed solution detected by high performance liquid chromatography (HPLC) was 0.03%.
[0056] (2) At 10-15°C, add 265g of dichloromethane to the protected meropenem feed solution obtained in step (1), and wash the organic phase three times with 200g of 10% sodium chloride solution respectively to obtain protected Meropenem organic phase material liqui...
Embodiment 2
[0068] A purification method for protecting meropenem, comprising the following steps:
[0069] (1) Add 140g of dichloromethane and 15g of meropenem side chains into the reaction flask, stir and dissolve to obtain a clear solution, add 25g of meropenem core to it, stir the solution until clear, cool to -25~-20°C, and 7.26 g of triethylamine was gradually added dropwise into the reaction flask, and after the dropwise addition was completed, the reaction was carried out at -25 to -20°C for 18 hours to obtain a protected meropenem feed solution.
[0070] The content of impurity IV in the side chain of meropenem was 45 ppm; the content of impurity V in the feed liquid detected by high performance liquid chromatography (HPLC) was 0.07%.
[0071] (2) Add 190 g of ethyl acetate to the protected meropenem feed solution obtained in step (1) at 10-15°C, and wash the organic phase three times with 200 g of deionized water respectively to obtain the protected meropenem organic phase feed ...
Embodiment 3
[0076] A purification method for protecting meropenem, comprising the following steps:
[0077] (1) Add 99.54g of N,N-dimethylformamide, 15g of meropenem side chain, 25g of meropenem nucleus and 2.6g of impurity IV into the reaction flask, stir the solution until it becomes clear, and cool down to -10~0℃ , 7.42g of N,N-diisopropylethylamine was gradually added dropwise into the reaction flask, and after the dropwise addition was completed, the reaction was carried out at -10 to 0°C for 20 hours to obtain a protected meropenem feed solution.
[0078] The content of impurity V in the feed liquid detected by high performance liquid chromatography (HPLC) was 19.70%.
[0079] (2) Add 265g of dichloromethane to the protected meropenem feed solution obtained in step (1) at 10-15°C, and wash the organic phase three times with 200g of 5% sodium acetate solution respectively to obtain protected meropenem Raopenem organic phase material liquid, concentrate the protected meropenem organi...
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