Process for preparing cefotaxime sodium
A cefotaxime sodium and a preparation process technology, applied in the field of compound preparation, can solve problems such as large amount of solvent used, poor crystallization condition, affecting product quality, etc., and achieve reduced amount of solvent used, low production cost, and low labor intensity Effect
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Embodiment 1
[0022] The preparation technology of cefotaxime sodium of the present invention is as follows:
[0023] Add 120ml of toluene and methanol at a volume ratio of 1:1 to form a mixed solvent, 20ml of triethylamine, cool down to 5°C, add 20g of 7-ACA, 28g of AE-active ester, and keep at 5°C for 60 Minutes, after the reaction is clarified, add sodium isooctanoate solution salt forming agent at room temperature, and 0.1g sodium bisulfite antioxidant, then add toluene dropwise to grow crystals for 30 minutes when it is slightly turbid, then add 150ml of toluene dropwise, and then add toluene dropwise The process can be properly cooled to 20°C, and the dripping is completed in 1.5 hours. After the dripping, the crystal is grown for 30 minutes and the material is discharged. The cake is washed with a mixture of 50ml ethyl acetate and 5ml absolute ethanol, and then the cake is added to 140ml acetone and Stir and wash in the mixed solution of 6ml of water for 30 minutes, then discharge th...
Embodiment 2
[0026] Add 130ml of toluene and methanol at a volume ratio of 1:1 to form a mixed solvent, 20ml of triethylamine, cool down to 6°C, add 20g of 7-ACA, 28g of AE-active ester, and keep at 6°C for 65 Minutes, after the reaction is clarified, add salt-forming agent and 0.1g sodium bisulfite antioxidant at room temperature, then add toluene dropwise to grow the crystal for 30 minutes when it is slightly turbid, then add 130ml of toluene dropwise, the temperature can be lowered to 22°C during the dropwise addition of toluene ℃, control the dropping in 2 hours, and feed the crystal for 30 minutes after the dropping, wash the cake with a mixture of 50ml ethyl acetate and 5ml absolute ethanol, and then add the cake to a mixture of 140ml acetone and 6ml water Stir and wash in the liquid for 30 minutes and discharge the material, then wash the material cake with a small amount of acetone, dry the wet product in vacuum at 50° C. for 3 hours, and collect 31.5 grams of dry product cefotaxime...
Embodiment 3
[0029] Add 130ml of toluene and methanol with a volume ratio of 1:1 to form a mixed solvent, 20ml of triethylamine, cool down to 7°C, add 20g of 7-ACA, 28g of AE-active ester, and keep at 8°C for 60 Minutes, after the reaction is clarified, add salt-forming agent and 0.09g sodium bisulfite antioxidant at room temperature, and then add toluene dropwise to grow the crystal for 30 minutes when it is slightly turbid, then add 140ml of toluene dropwise, and the temperature can be lowered to 18% during the dropwise addition of toluene ℃, controlled at 1.7 hours to finish dropping, after dropping, grow the crystal for 30 minutes and discharge the material, wash the cake with a mixture of 50ml ethyl acetate and 5ml methanol, and then add the cake to a mixture of 120ml acetone and 3ml water Stir and wash for 30 minutes and discharge, then wash the cake with a small amount of acetone, dry the wet material under vacuum at 50° C. for 3 hours, and collect 31.7 g of dry product cefotaxime so...
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