Hosztafi S, Répási J
Alkaloida Vegyészeti Gyár Rt., Tiszavasvári.
Acta Pharm Hung. 1994 Jan;64(1):22-5.
Dansyl derivatives of morphine-like substances were prepared using dansyl-chloride in acetone in the presence of sodium hydrogen carbonate. The reaction was selective for the phenolic hydroxyl group and was also quantitative. The purity of crystalline dansyl derivatives was checked by thin layer chromatography. Their structure was confirmed by PMR and MS spectra. Characteristic chemical shifts and MS fragments of the new derivatives were determined. UV spectra of the parent compounds and the dansyl derivatives were recorded. It was found that the absorbance of dansyl derivatives at 286 nm increased four-fold and a new band appeared at 320 nm. Some thin-layer chromatographic systems were elaborated to detect and separate dansyl derivatives. HPLC studies were done using normal as well as reversed phase. Parent compounds and their dansyl derivatives were separated easily by HPLC.
在碳酸氢钠存在下,于丙酮中使用丹磺酰氯制备吗啡样物质的丹磺酰衍生物。该反应对酚羟基具有选择性且是定量的。通过薄层色谱法检查结晶丹磺酰衍生物的纯度。通过核磁共振氢谱(PMR)和质谱(MS)光谱确认其结构。测定了新衍生物的特征化学位移和质谱碎片。记录了母体化合物和丹磺酰衍生物的紫外光谱。发现丹磺酰衍生物在286 nm处的吸光度增加了四倍,并且在320 nm处出现了一个新的谱带。精心设计了一些薄层色谱系统来检测和分离丹磺酰衍生物。使用正相和反相进行了高效液相色谱(HPLC)研究。母体化合物及其丹磺酰衍生物通过HPLC很容易分离。