A kind of preparation method of cefpirome sulfate
A technology of cefpirome sulfate and ethyl acetate, which is applied in the field of preparation of cefpirome sulfate, can solve the problems of high water content, low water content, low product purity, etc., and achieve low color index, small water content and high stability Good results
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Embodiment 1
[0019] a) Add 20 g of cefpirome sulfate crude product into 70 ml of ethyl acetate aqueous solution, and the volume ratio of ethyl acetate to water in the ethyl acetate aqueous solution is 1:0.8. The temperature was lowered to 5° C., and NaOH solution was added to the solution under stirring until all the solids were dissolved to obtain a solution.
[0020] b) Add 72.7mL of acetone to the solution, adjust the pH value of the solution to 4.4-4.2 with 40% sulfuric acid solution to prepare an acidic mixture, then add 0.45g of activated carbon and 0.7g of Sodium sulfite was used for decolorization treatment for 15 minutes, and after the decolorization treatment was completed, it was filtered, the filter cake was washed with purified water, and the filtrate was collected.
[0021] c) performing aseptic filtration on the filtrate with a microfiltration membrane to obtain a sterile filtrate; the pore size of the microfiltration membrane is 0.3 μm.
[0022] d) Warm up the sterile filt...
Embodiment 2
[0025] a) Add 20 g of cefpirome sulfate crude product to 70 ml of ethyl acetate aqueous solution, and the volume ratio of ethyl acetate to water in the aqueous solution is 1:1. The temperature was lowered to 5° C., and ammonia water was added to the solution under stirring until all the solids were dissolved to obtain a solution.
[0026] b) Add 97.0mL of acetone to the solution, adjust the pH value of the solution to 4.4-4.2 with 40% sulfuric acid solution to prepare an acidic mixture, then add 0.7g of activated carbon and 0.5g of Sulfurous acid, carry out decolorization treatment for 20min, filter after completion of decolorization treatment, wash the filter cake with purified water, and collect the filtrate.
[0027] c) performing aseptic filtration on the filtrate with a microfiltration membrane to obtain a sterile filtrate; the pore size of the microfiltration membrane is 0.45 μm.
[0028] When the sterile filtrate becomes turbid, grow the crystals for 2 hours, then add ...
Embodiment 3
[0031] a) Add 20 g of cefpirome sulfate crude product to 70 ml of ethyl acetate aqueous solution, and the volume ratio of ethyl acetate to water in the aqueous solution is 1:1.2. The temperature was lowered to 5°C, and sodium bicarbonate solution was added to the solution under stirring until all the solids were dissolved to obtain a solution.
[0032] b) Add 121.3mL of acetone to the solution, adjust the pH value of the solution to 4.4-4.2 with 40% sulfuric acid solution to prepare an acidic mixed solution, then add 1g of activated carbon and 0.4g of sulfuric acid to the acidic mixed solution Sodium bisulfate was used for decolorization treatment for 30 minutes, after the decolorization treatment was completed, it was filtered, the filter cake was washed with purified water, and the filtrate was collected.
[0033] c) performing aseptic filtration on the filtrate with a microfiltration membrane to obtain a sterile filtrate; the pore size of the microfiltration membrane is 0.6...
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