Method for preparing high-purity cefpodoxime proxetil
A technology of cefpodoxime axetil and cefpodoxime acid, which is applied in the field of preparing high-purity cefpodoxime axetil, can solve the problems of low yield and expensive quaternary ammonium salt, and achieve high yield, easy operation and good product stability Effect
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[0028] Example 1
[0029] Put 10g (0.0234moL) cefpodoxime B into 50ml DMAc (N,N-dimethylacetamide) in a 250ml reaction flask under nitrogen protection, stir and cool to -20℃ to dissolve, add [bmlm] OH 0.05g, potassium carbonate 3.5g, stirred for 20 minutes. Add 6.5g (0.0253mol) of isopropyl α-iodoethyloxycarbonate dropwise, control the temperature at -18℃~-19℃, after 30 minutes of reaction, HPLC control the raw material cefpodoximate B≤0.5%, esterification reaction At the end, add 1g of medicinal activated carbon for decolorization. After decolorization, slowly press the esterification reactant into 400ml of 1% methanol / purified aqueous solution that has been cooled to 5°C. After pressure filtration, continue to stir for 30 minutes. The product was washed with 50 mL of water and dried in vacuum to obtain 10.5 g of a white powder solid (molar yield 80.6%).
[0030] Product (R+S)HPLC=99.2%, R / (R+S)=0.51, Δ 3 = 0.35%.
Example Embodiment
[0031] Example 2
[0032] Put 10g (0.0234moL) cefpodoxime B into 50ml DMAc in a 250ml reaction flask under nitrogen protection, stir and cool to -20℃ to dissolve, add [bmlm]OH0.1g, sodium carbonate 3.1g and stir for 20 minutes . Add dropwise α-iodoethyl oxyisopropyl carbonate (6.5g 0.0253mol), control the temperature at -18℃~-19℃, and react for 30 minutes,
[0033] HPLC control raw material cefpodoxime B≤0.5%, the esterification reaction is over, add 1g of medicinal activated carbon for decolorization, after decolorization, slowly press the esterification reactant into the 1% methanol / purified water solution which has been cooled to 5℃ in advance In 400 ml, after the pressure filtration, continue to stir for 30 minutes, and then shake the filter, wash the product with 50 ml of purified water, and dry in vacuum to obtain 10.2 g of white powder solid (molar yield=78.3%).
[0034] Product (R+S) HPLC=99.1%, R / (R+S)=0.53, Δ3=0.36%.
Example Embodiment
[0035] Example 3
[0036] Put 20g (0.0468moL) cefpodoxime B into 100ml DMF in a 250ml four-neck flask under nitrogen protection, stir and cool to -15℃~-18℃ to dissolve, add [bmlm]OH0.2g, potassium carbonate 6.3 g, stirring for 20 minutes. Add 13 g (0.0505 mol) of α-iodoethyl isopropyl oxycarbonate, after 30 minutes of heat preservation and reaction, HPLC controls the raw material cefpodoxime B ≤ 0.5%, the esterification reaction is over, and 2 g of medicinal activated carbon is added for decolorization and decolorization After completion, slowly press the esterification reactant into 800 ml of 2% ethanol / purified aqueous solution which has been cooled to 5° C., after the pressure filtration is completed, a solid is precipitated, and the stirring is continued for 30 minutes. Spin filtration, washing with 50 mL of purified water, and vacuum drying to obtain 18.9 g of white powder solid (weight yield = 94.5%).
[0037] Product (R+S) HPLC=99.2%, R / (R+S)=0.51, Δ 3 = 0.37%.
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