The 7 (phenylacetamido)deacetoxycephalosporin acid was prepared by ring expansion of penicillin G sulfoxide via its trimethylsiliated intermediate(protective silylation with N,N dimethylsilylurea) using HBr 4 methy...The 7 (phenylacetamido)deacetoxycephalosporin acid was prepared by ring expansion of penicillin G sulfoxide via its trimethylsiliated intermediate(protective silylation with N,N dimethylsilylurea) using HBr 4 methylpyridine as catalyst. The effects of catal yst amount, reaction temperature and time were examined. Under optimum reaction condi tions product in 94% yield was obtained. The product has been characterized by IR and MS.展开更多
The preparation procedure of benzylpenicillin sulfoxide p-methoxybenzyl ester by esterificating penicillin G potassium salt and following oxidizing the corresponding benzylpenicillin ester is described. The method usi...The preparation procedure of benzylpenicillin sulfoxide p-methoxybenzyl ester by esterificating penicillin G potassium salt and following oxidizing the corresponding benzylpenicillin ester is described. The method using the only reactive solvent minimizes the kinds of solvents and decreases the volume of solvents, which facilitates technical procedures and reduces the cost.展开更多
建立高效液相色谱-二极管阵列检测器法测定青霉素亚砜酯的含量。采用Agilent Eclipse Plus C18(3.0 mm×100 mm, 3.5μm)色谱柱;柱温30℃;以25 mmol·L^-1的醋酸铵水溶液(A)-乙腈(B)为流动相进行梯度洗脱;流速为0.5 mL·min...建立高效液相色谱-二极管阵列检测器法测定青霉素亚砜酯的含量。采用Agilent Eclipse Plus C18(3.0 mm×100 mm, 3.5μm)色谱柱;柱温30℃;以25 mmol·L^-1的醋酸铵水溶液(A)-乙腈(B)为流动相进行梯度洗脱;流速为0.5 mL·min^-1;检测波长267 nm。青霉素亚砜酯在0.01~0.80 mg·mL^-1(R^2=0.999 9)范围内线性较好,精密度RSD为0.15%。方法操作简单,结果准确,特异性强,稳定性好,适用于青霉素亚砜酯的含量测定。展开更多
文摘The 7 (phenylacetamido)deacetoxycephalosporin acid was prepared by ring expansion of penicillin G sulfoxide via its trimethylsiliated intermediate(protective silylation with N,N dimethylsilylurea) using HBr 4 methylpyridine as catalyst. The effects of catal yst amount, reaction temperature and time were examined. Under optimum reaction condi tions product in 94% yield was obtained. The product has been characterized by IR and MS.
文摘The preparation procedure of benzylpenicillin sulfoxide p-methoxybenzyl ester by esterificating penicillin G potassium salt and following oxidizing the corresponding benzylpenicillin ester is described. The method using the only reactive solvent minimizes the kinds of solvents and decreases the volume of solvents, which facilitates technical procedures and reduces the cost.
