Several novel macrocyclic arenes that are composed of six indole subunits,so-called bisindole[3]arenes(BID[3]s),were conveniently synthesized by the aluminum trichloride-catalyzed one-pot condensation of bisindole der...Several novel macrocyclic arenes that are composed of six indole subunits,so-called bisindole[3]arenes(BID[3]s),were conveniently synthesized by the aluminum trichloride-catalyzed one-pot condensation of bisindole derivatives and paraformaldehyde in dichloromethane at room temperature.Their macrocyclic structures were demonstrated by X-ray single-crystal studies,and the presence of the macrocyclic cavities made it possible to accommodate specific small organic molecules.The BID[3]s have exceptionally high iodine adsorption ability due to the strong and synergic interaction of indole units toward iodine,exhibiting significant morphology changes upon adsorption and desorption of iodine.Iodine uptake capacity of up to 5.12 g·g^(−1) was found with MeBID[3],which is the highest value ever reported for macrocyclic arenes.展开更多
AIM:To establish a method to simultaneously determine the main five alkaloids of Catharanthus roseus for trace samples,a high-performance liquid chromatography–electrospray ionization-tandem mass spectrometry(HPLC-ES...AIM:To establish a method to simultaneously determine the main five alkaloids of Catharanthus roseus for trace samples,a high-performance liquid chromatography–electrospray ionization-tandem mass spectrometry(HPLC-ESI-MS/MS)analysis method was developed.METHOD:The five Catharanthus alkaloids,vinblastine,vincristine,vinleurosine,vindoline,and catharanthine were chromatographically separated on a C18 HPLC column.The mobile phase was methanol-15 nmol?L–1 ammonium acetate containing 0.02%formic acid(65:35,V/V).The quantification of these alkaloids was based on the Multiple Reaction Monitoring(MRM)mode.RESULTS:This method was validated,and the results achieved the aims of the study.The intra-and inter-day precision and accuracy of the five alkaloids were within 1.2%-11.5%(RSD%)and-10.9%-10.5%(RE%).The recovery rates of the five alkaloids of samples were from 79.9%to 91.5%.The five analytes were stable at room temperature for 2 h,at 4°C for 12 h,and at-20°C for two weeks.The developed method was applied successfully to determine the content of the five alkaloids in three plant parts of three batches of C.roseus with a minute amount collected from three regions of China.CONCLUSION:The HPLC-ESI-MS/MS method can be used for the simultaneous determination of five important alkaloids in trace C.roseus samples.展开更多
An efficient regioselective Friedel-Crafts hydroxyalkylation of N-substituted glyoxylamide with various indoles catalyzed by Lewis acids was developed. The reactions proceeded smoothly at room temperature and the 2-hy...An efficient regioselective Friedel-Crafts hydroxyalkylation of N-substituted glyoxylamide with various indoles catalyzed by Lewis acids was developed. The reactions proceeded smoothly at room temperature and the 2-hydroxy-2-（1H-indol-3-yl）-N-substituted acetamide resulted from the reactions catalyzed by FeSO4 were synthesized in excellent yields （up to 93%）. While the bisindole compounds were obtained when FeCl3 was used as a catalyst in excellent yields （up to 92%）. A possible mechanism was proposed.展开更多
基金supported by the National Natural Science Foundation of China(nos.21871194,21971169,and 21572142)National Key Research and Development Program of China(no.2017YFA0505903).
文摘Several novel macrocyclic arenes that are composed of six indole subunits,so-called bisindole[3]arenes(BID[3]s),were conveniently synthesized by the aluminum trichloride-catalyzed one-pot condensation of bisindole derivatives and paraformaldehyde in dichloromethane at room temperature.Their macrocyclic structures were demonstrated by X-ray single-crystal studies,and the presence of the macrocyclic cavities made it possible to accommodate specific small organic molecules.The BID[3]s have exceptionally high iodine adsorption ability due to the strong and synergic interaction of indole units toward iodine,exhibiting significant morphology changes upon adsorption and desorption of iodine.Iodine uptake capacity of up to 5.12 g·g^(−1) was found with MeBID[3],which is the highest value ever reported for macrocyclic arenes.
基金supported by the Fundamental Research Funds for the Central Universities(No.DL09BA21)Special Fund for Forestry Scientific Research in the Public Interest(No.201204601)
文摘AIM:To establish a method to simultaneously determine the main five alkaloids of Catharanthus roseus for trace samples,a high-performance liquid chromatography–electrospray ionization-tandem mass spectrometry(HPLC-ESI-MS/MS)analysis method was developed.METHOD:The five Catharanthus alkaloids,vinblastine,vincristine,vinleurosine,vindoline,and catharanthine were chromatographically separated on a C18 HPLC column.The mobile phase was methanol-15 nmol?L–1 ammonium acetate containing 0.02%formic acid(65:35,V/V).The quantification of these alkaloids was based on the Multiple Reaction Monitoring(MRM)mode.RESULTS:This method was validated,and the results achieved the aims of the study.The intra-and inter-day precision and accuracy of the five alkaloids were within 1.2%-11.5%(RSD%)and-10.9%-10.5%(RE%).The recovery rates of the five alkaloids of samples were from 79.9%to 91.5%.The five analytes were stable at room temperature for 2 h,at 4°C for 12 h,and at-20°C for two weeks.The developed method was applied successfully to determine the content of the five alkaloids in three plant parts of three batches of C.roseus with a minute amount collected from three regions of China.CONCLUSION:The HPLC-ESI-MS/MS method can be used for the simultaneous determination of five important alkaloids in trace C.roseus samples.
基金the National Natural Science Foundation of China (Nos. 21472130, 81373259) for financial support of this study
文摘An efficient regioselective Friedel-Crafts hydroxyalkylation of N-substituted glyoxylamide with various indoles catalyzed by Lewis acids was developed. The reactions proceeded smoothly at room temperature and the 2-hydroxy-2-（1H-indol-3-yl）-N-substituted acetamide resulted from the reactions catalyzed by FeSO4 were synthesized in excellent yields （up to 93%）. While the bisindole compounds were obtained when FeCl3 was used as a catalyst in excellent yields （up to 92%）. A possible mechanism was proposed.
