Cefdinir impurity mixture and preparation method thereof
A technology of cefdinir and its mixture, which is applied in the field of cefdinir impurity mixture and its preparation, can solve problems such as uneven quality, achieve the effects of reducing process steps, mild reaction conditions, and meeting the needs of quality research
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Embodiment 1
[0035] A preparation method for the mixture of cefdinir impurity I and cefdinir impurity J, comprising the following steps:
[0036] (1) Weigh 5g of cefdinir raw material, dissolve it in 300ml of pure water, adjust the pH of the reaction solution to 11.0 with NaOH solid particles and react for about 24 hours, then adjust the pH to 7.0 with phosphoric acid to obtain the purity cefdinir impurity 1, and separate it with C18 material Separation on a chromatographic column, elution with pure water, detection by HPLC, and collection of the eluted part with pure water, to obtain cefdinir impurity 1 with a purity of 90%;
[0037] (2) Synthesis of the mixture of cefdinir impurity I and cefdinir impurity J: take cefdinir impurity 1 with a purity of 90%, adjust pH=3.0 with phosphoric acid, and react at 4°C for about 4 hours in refrigeration to obtain low-purity The mixture of cefdinir impurity I and cefdinir impurity J was separated by a C18 material separation chromatographic column, el...
Embodiment 2
[0039] A preparation method for the mixture of cefdinir impurity I and cefdinir impurity J, comprising the following steps:
[0040] (1) Weigh 5g of cefdinir raw material, dissolve it in 300ml of pure water, adjust the pH of the reaction solution to 10.5 with NaOH solid particles and react for about 24h, then adjust the pH to 6.5 with phosphoric acid to obtain the purity cefdinir impurity 1, and separate it with C18 material Separation on a chromatographic column, elution with pure water, detection by HPLC, and collection of the eluted part with pure water to obtain cefdinir impurity 1;
[0041] (2) Synthesis of cefdinir impurity I and cefdinir impurity J mixture: take cefdinir impurity 1 with a purity of 90%, adjust pH=2.5 with phosphoric acid, and react for about 4 hours at 5°C in refrigeration to obtain low-purity The mixture of cefdinir impurity I and cefdinir impurity J is separated by C18 material separation chromatographic column, eluted with acid water with pH=5.0 and ...
Embodiment 3
[0043] A preparation method for the mixture of cefdinir impurity I and cefdinir impurity J, comprising the following steps:
[0044](1) Weigh 5g of cefdinir raw material, dissolve it in 300ml of pure water, adjust the pH of the reaction solution to 11.5 with NaOH solid particles, react for about 10h, and adjust the pH to 7.5 with phosphoric acid to obtain the purity cefdinir impurity 1, which is separated with C18 material Separation on a chromatographic column, elution with pure water, detection by HPLC, and collection of the eluted part with pure water to obtain cefdinir impurity 1;
[0045] (2) Synthesis of the mixture of cefdinir impurity I and cefdinir impurity J: take cefdinir impurity 1 with a purity of 90%, adjust pH=3.5 with phosphoric acid, and react for about 4 hours at 3°C in refrigeration to obtain low-purity The mixture of cefdinir impurity I and cefdinir impurity J is separated by C18 material separation chromatographic column, eluted with acid water with pH=5...
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