Phosphorylation cephalosporin derivates
A compound, phosphono technology, applied in the field of medicine, can solve the problems of strong bacterial resistance and affecting the antibacterial efficacy of cephalosporins
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Embodiment 1
[0092] Embodiment 1 Preparation of Compound 1 of the present invention and its sodium salt
[0093] Step 1: Preparation of diisopropyl phosphite
[0094] Add 240ml of anhydrous isopropanol and 40ml of toluene into a 500ml four-necked bottle, control the temperature in an ice-water bath below 15°C, and add 70ml of phosphorus trichloride (PCl 3 ) within 4 hours, the temperature was raised to 50-60°C, and the reaction was continued for 6 hours. At the same time, the hydrogen chloride gas generated in the system was extracted under reduced pressure, concentrated under reduced pressure, and the concentrated liquid was rectified, collected at 62-67°C / 0.095 The fraction of MP can be obtained.
[0095] Step 2: Preparation of compound 1 of the present invention
[0096] Under ice-salt bath, control the temperature at about 0°C, add 26.5g (45mmol) of cefodizime acid into a 1000ml four-neck bottle, add 200ml of water, stir, adjust the pH to 9.5 with 25% sodium hydroxide solution, and...
Embodiment 2
[0107] Embodiment 2 Preparation of Compound 2 of the present invention and its sodium salt
[0108] Step 1: Preparation of diethyl phosphite
[0109] Add 230ml of absolute ethanol and 50ml of carbon tetrachloride into a 1000ml four-necked bottle, control the temperature in an ice-water bath below 15°C, and add 88ml of phosphorus trichloride (PCl 3 ) was added within 4 hours, heated to 50-60°C, and continued to react for 6 hours. At the same time, the hydrogen chloride gas generated in the system was extracted under reduced pressure, concentrated under reduced pressure, and the concentrated liquid was rectified, collected at 89-93°C / 0.095 The fraction of MP can be obtained.
[0110] Step 2: Preparation of compound 2 of the present invention
[0111] Under ice-salt bath, control the temperature at about 0°C, add 26.5g (45mmol) of cefodizime acid into a 1000ml four-neck bottle, add 200ml of water, stir, adjust the pH to 9.5 with 25% sodium hydroxide solution, and the solids a...
Embodiment 3
[0122] Embodiment 3 Preparation of Compound 3 of the present invention and its sodium salt
[0123] Step 1: Preparation of compound 3 of the present invention
[0124] Under ice-salt bath, control the temperature at about 0°C, add 26.5g (45mmol) of cefodizime acid into a 1000ml four-neck bottle, add 200ml of water, stir, adjust the pH to 9-10 with 25% sodium hydroxide solution, solid Completely dissolve, add 108mg tetrabutylammonium bromide and 4.2g (50mmol) phosphorous acid, dropwise add 22.5ml concentration and be 12% sodium hypochlorite solution. After addition, the reaction was continued for 4 hours. Stop the reaction, add diethyl ether to extract once, lower the pH of the aqueous layer to 3 with hydrochloric acid in an ice bath, freeze and crystallize, filter, wash the filter cake with ethanol, filter, and dry the filter cake at 40°C for 8 hours under reduced pressure to obtain a light yellow powder 26.5 g, yield: 78.5%.
[0125] Molecular formula: C 20 h 21 N 6 o...
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