Pharmaceutical preparation of cefoxitin sodium compound and its application in prevention of infection before vaginal hysterectomy, abdominal hysterectomy and caesarean section (uterine) delivery
A technology of cefoxitin sodium and cefalotin acid, which is applied in organic chemistry, pharmaceutical formulations, antibacterial drugs, etc., to achieve the effects of good quality stability, simplified processing steps, and uniform particle size range
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[0044] The invention provides a kind of preparation method of cefoxitin sodium or its composition, and described preparation method comprises the following steps:
[0045] Step 1: dissolving 7-aminocephalosporanic acid (7-ACA) in the reaction solvent, adding a phase transfer catalyst and an alkaline solution, adding thiopheneacetyl chloride dropwise under temperature control, and filtering to obtain cephalothinic acid after the reaction;
[0046] Step 2: After the cephalotinic acid is dissolved, it reacts with the sodium methoxide solution added dropwise, and after the reaction solution is treated, it forms a salt with an organic base for purification to obtain an organic alkali salt of 7-methoxycephalothinic acid.
[0047] Step 3: Dissolving 7-methoxycephalothinic acid cyclohexylamine salt in methanol-water solution, adding an aqueous inorganic alkali solution dropwise after cooling down, adjusting the acid after the reaction, stirring, and crystallizing to obtain a deacetylat...
Embodiment 1
[0169] Step 1: In a 10L four-necked round bottom flask, add 500g of 7-aminocephalosporanic acid (7-ACA) and 5000ml of dichloromethane, and add 170g of sodium bicarbonate saturated aqueous solution and 5.0g of tetrabutyl bromide under stirring Ammonium chloride, temperature control -5 ~ 0 ° C, dropwise added 308g thiophene acetyl chloride, control in 50 ~ 60 minutes to complete the dropwise addition. After incubation and reaction for 4 hours, filter, wash the filter cake with dichloromethane, filter with suction, and dry to obtain cephalothinic acid.
[0170] Step 2: Add 5000ml of dichloromethane, 800ml of tetrahydrofuran and 600g of cephalothinic acid into a 10L four-neck round bottom flask, stir to completely dissolve and cool down to -60°C, add dropwise methanol solution containing 126g of sodium methoxide within 60 minutes, Mass concentration is 30%, after adding, continue to stir for 45 minutes, then dropwise add 181g tert-butyl hypochlorite, finish adding in 45 minutes, i...
Embodiment 2
[0175] Step 1: In a 10L four-neck round bottom flask, add 500g of 7-aminocephalosporanic acid (7-ACA) and 5000ml of dichloromethane, and add a saturated aqueous solution of 200g of sodium bicarbonate and 7.5g of tetrabutyl bromide under stirring ammonium chloride, temperature controlled at -5 to -3°C, 308g of thiopheneacetyl chloride was added dropwise, and the dropwise addition was completed within 50 to 60 minutes. After incubation and reaction for 3 hours, filter, wash the filter cake with dichloromethane, filter with suction, and dry to obtain cephalothinic acid.
[0176] Step 2: Add 5000ml of dichloromethane, 1000ml of tetrahydrofuran and 600g of cephalothinic acid into a 10L four-neck round bottom flask, stir to completely dissolve and cool down to -50°C, add dropwise methanol solution containing 122.4g of sodium methoxide within 60 minutes, sodium methoxide The mass concentration is 25%, after adding, continue to stir for 45 minutes, then dropwise add 164g tert-butyl hy...
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