A kind of preparation method of 3-ethyl cefadroxil
A technology of ethyl cefadroxil and acylation, which is applied in the field of preparation of 3-ethyl cefadroxil, can solve the problems of reducing the curative effect of drugs, complicated production process of cefadroxil, human harm and the like, and achieves strong operability, The effect of high purity and high yield
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Embodiment 1
[0027] Synthesis of compound Ⅱ
[0028] The reaction process is:
[0029]
[0030] Get 50 grams of 7-amino-3-vinyl-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid (7-AVCA) suspended at 290 Add 54 ml of boron trifluoride diethyl ether slowly to the above solution in an ice bath, and react at 20°C for 6 hours to obtain a clear yellow solution. The reaction solution is slowly quenched with saturated sodium carbonate solution to neutral partial Alkaline (pH=9), suction filter the quenched reaction solution, extract the filtrate 3 times with 200 ml ethyl acetate, combine the organic phases, wash 3 times with 100 ml saturated brine, and wash the organic phase with anhydrous sodium sulfate Dry, filter and spin dry to obtain crude product. The crude product was slurried with 300 ml of n-hexane to obtain compound II, 49.12 g, off-white solid, yield 78.7%.
[0031] Compound Ⅱ structural characterization results: 1 H-NMR (DMSO-d 6 )δppm: 6.72-6.79(dd,1H),5.53-5.57(d,1...
Embodiment 2
[0053] Synthesis of compound Ⅱ
[0054] The reaction process is:
[0055]
[0056] Take 10 grams of 7-amino-3-vinyl-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid (7-AVCA) suspended in 150 In one milliliter of N,N-dimethylformamide, add 8.82 grams of sodium isooctanoate to the above reaction solution, then react at room temperature for 30 minutes to obtain a clear solution, add 12.1 grams of tert-butyl bromide to the reaction solution, and continue to react at room temperature for 12 hours , a yellow solution was obtained. Add 300 ml of water to the reaction solution, and extract 3 times with 150 ml of ethyl acetate, combine the organic phases, wash 3 times with 200 ml of saturated brine, dry the organic phase with anhydrous sodium sulfate, filter and spin dry to obtain a crude product. The crude product was purified once by column chromatography to obtain compound II, 3.8 g of off-white solid, with a yield of 30.4%.
[0057] Compound Ⅱ structural characteri...
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