A kind of synthetic method of antibiotic cephalosporin nuclei
A synthesis method and technology for antibiotics are applied in the synthesis field of antibiotic cephalosporins, can solve problems such as low yield, high cost of raw materials, can not meet market demands, etc., achieve high product yield, improve solubility, reduce production costs and The effect of labor intensity
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Embodiment 1
[0048] (1) Preparation of reaction solution I: Weigh 53.4g GCLH in a 500ml three-necked flask (with thermometer, mechanical stirring), add 200ml acetonitrile, then add 28.8g triphenylphosphine, 11.3g sodium bromide, and then add 30% hydrochloric acid 1.1 g, heat up to 35°C, keep the temperature for 2 hours, and control the GCLH in the reaction solution to <1% by HPLC to obtain the reaction solution I, which contains compound 1;
[0049] (2) Preparation of reaction solution II: Cool the reaction solution I to zero, add 40% formaldehyde, then add (0.03mol) potassium carbonate / sodium hydroxide (0.08mol) mixed solution, and react at 5°C for 3 hours , HPLC control compound 1<0.5%, obtain reaction solution II, containing compound 2 in reaction solution II;
[0050] (3) Preparation of compound GVNA: Distill the reaction solution II under reduced pressure, control the temperature at 45° C., recover acetonitrile, precipitate a white solid, filter, put the obtained filter cake into 300 ...
Embodiment 2
[0053] (1) Preparation of reaction solution I: Weigh 50.2g GCLH in a 500ml three-neck flask (with thermometer, mechanical stirring), add 200ml acetone, then add 28.5g triphenylphosphine, 10.9g sodium bromide, and then add 40% hydrogen 1.1 g of bromic acid, heated up to 38° C., kept the temperature for 2.5 hours, and controlled GCLH<1% in the reaction solution by HPLC to obtain reaction solution I, which contained compound 1;
[0054] (2) Cool the reaction solution I to zero, add 40% formaldehyde, and then add (0.03mol) potassium carbonate / sodium hydroxide (0.08mol) mixed solution, control the temperature at 8°C for 2.5 hours, HPLC control compound 1< 0.5%, to obtain reaction solution II, which contains compound 2;
[0055] (3) Preparation of compound GVNA: The reaction solution II was distilled under reduced pressure, and the temperature was controlled at 47°C. After recovering acetone, a white solid was precipitated, filtered, and the obtained filter cake was put into 400ml o...
Embodiment 3
[0058] (1) Preparation of reaction solution I: Weigh 51.2g GCLH in a 500ml three-neck flask (with thermometer, mechanical stirring), add 200ml acetone, then add 28.3g triphenylphosphine, 11.1g sodium bromide, and then add 35% nitric acid 1.1 g, heat up to 40°C, keep the temperature for 3 hours, and control the GCLH in the reaction solution to <1% by HPLC to obtain the reaction solution I, which contains compound 1;
[0059] (2) Preparation of reaction solution II: cool the reaction solution I to zero, add 40% formaldehyde, then add (0.03mol) potassium carbonate / sodium hydroxide (0.08mol) mixed solution, and control the temperature at 10°C for 2 hours , HPLC control compound 1<0.5%, obtain reaction solution II, containing compound 2 in reaction solution II;
[0060] (3) Preparation of compound GVNA: The reaction solution II was distilled under reduced pressure, and the temperature was controlled at 50° C. After recovering acetone, a white solid was precipitated, filtered, and t...
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