A detailed analysis of benzofuranone compounds under multiple tandem mass spectrometry （ESI-MS^n） conditions is reported. Element composition data of the fragment ions were obtained with the aid of comparison of the...A detailed analysis of benzofuranone compounds under multiple tandem mass spectrometry （ESI-MS^n） conditions is reported. Element composition data of the fragment ions were obtained with the aid of comparison of the multiple tandem mass spectra of four compounds, and the structures of which are identical except for some substituted groups or epimers or cis-trans-isomers. Attempts have been made to provide rational pathways for the formation of the fragment ions from these protonated compounds. And the structure-fragmentation relationships will facilitate the characterization of the structures of other analogs.展开更多
Aim To establish the method for determination of benzofuranones derivative, griffonilide, in the roots of Semiaquilegia adoxoides （DC.） Makino by RP- HPLC. Methods Kromasil C18 column was used with a mobile phase of...Aim To establish the method for determination of benzofuranones derivative, griffonilide, in the roots of Semiaquilegia adoxoides （DC.） Makino by RP- HPLC. Methods Kromasil C18 column was used with a mobile phase of methanol-water （ containing 0. 01% trifluoroacetic acid and 0. 05 % tetrahydrofuran） （3：97）. The detecting wavelength was 260 nm. Results The calibration curve was linear over the range of 0. 004 - 0. 4 mg·mL^-1 with the correlation coefficient of 1.00 000. The average recovery was 98. 77 % with RSD 2. 77 %. Determinations of ten samples from different areas showed that the contents of griffonilide in the roots of S. adoxoides are 0. 17 -0. 49 mg·g^-1. Conclusion The method provides an accurate and sensitive way to detect griffonilide in the roots of S. adoxoides .展开更多
The enantioselective double Michael reaction of benzofuranone with dienones catalyzed by Cinchona-based primary amines was developed. A number of optically active spirocyclic benzofuranones were obtained in up to 89% ...The enantioselective double Michael reaction of benzofuranone with dienones catalyzed by Cinchona-based primary amines was developed. A number of optically active spirocyclic benzofuranones were obtained in up to 89% yield and 91% ee.展开更多
采用高效液相色谱仪建立了测定苯并呋喃酮的定量定性分析方法。采用C18不锈钢柱(150 mm×4.6 mm i.d.,5μm)和二极管阵列检测器,乙腈、甲醇和0.1%磷酸水溶液为流动相,梯度洗脱,在268 nm波长下对苯并呋喃酮进行分离和定量分析。结果...采用高效液相色谱仪建立了测定苯并呋喃酮的定量定性分析方法。采用C18不锈钢柱(150 mm×4.6 mm i.d.,5μm)和二极管阵列检测器,乙腈、甲醇和0.1%磷酸水溶液为流动相,梯度洗脱,在268 nm波长下对苯并呋喃酮进行分离和定量分析。结果表明,该方法测得苯并呋喃酮的保留时间为10.1 min,线性相关系数为0.9999,标准偏差为0.09,变异系数为0.13%,平均回收率为100.02%。该方法具有操作简便、快速稳定、结果准确等特点,可满足苯并呋喃酮生产过程中的定量分析和质量控制要求。展开更多
A quinine-derived thiourea-catalyzed inter-/intramolecular Michael cycloaddition of chromoneoxindole/benzofuranone synthons with 3-substituted methylenebenzofuranones has been established,which constructed enantiomeri...A quinine-derived thiourea-catalyzed inter-/intramolecular Michael cycloaddition of chromoneoxindole/benzofuranone synthons with 3-substituted methylenebenzofuranones has been established,which constructed enantiomerically pure bispiro[benzofuran-oxindole/benzofuran-chromanone]s bearing five consecutive stereocenters including two spiro quaternary carton centers in good yields(up to 93%) with high diastereoselectivities(up to>20:1 dr) and good enantioselectivities(up to>99% ee).Moreover,this is the first example of bifunctional chromone-benzofuranone synthon directed organocatalytic tandem reaction,and also the first example of the bispiro[benzofuran-oxindole] and bispirobenzofuranone,potentially useful in medicinal chemistry.展开更多
文摘A detailed analysis of benzofuranone compounds under multiple tandem mass spectrometry （ESI-MS^n） conditions is reported. Element composition data of the fragment ions were obtained with the aid of comparison of the multiple tandem mass spectra of four compounds, and the structures of which are identical except for some substituted groups or epimers or cis-trans-isomers. Attempts have been made to provide rational pathways for the formation of the fragment ions from these protonated compounds. And the structure-fragmentation relationships will facilitate the characterization of the structures of other analogs.
基金Ministry of Science and Technology of People'sRepublic of China (No. 2004AA2Z3730)
文摘Aim To establish the method for determination of benzofuranones derivative, griffonilide, in the roots of Semiaquilegia adoxoides （DC.） Makino by RP- HPLC. Methods Kromasil C18 column was used with a mobile phase of methanol-water （ containing 0. 01% trifluoroacetic acid and 0. 05 % tetrahydrofuran） （3：97）. The detecting wavelength was 260 nm. Results The calibration curve was linear over the range of 0. 004 - 0. 4 mg·mL^-1 with the correlation coefficient of 1.00 000. The average recovery was 98. 77 % with RSD 2. 77 %. Determinations of ten samples from different areas showed that the contents of griffonilide in the roots of S. adoxoides are 0. 17 -0. 49 mg·g^-1. Conclusion The method provides an accurate and sensitive way to detect griffonilide in the roots of S. adoxoides .
基金Acknowledgement This work was supported by National Natural Science Foundation of China （Nos. 20802075 and No. 21042006）.
文摘The enantioselective double Michael reaction of benzofuranone with dienones catalyzed by Cinchona-based primary amines was developed. A number of optically active spirocyclic benzofuranones were obtained in up to 89% yield and 91% ee.
基金financial support from the National Nature Science Foundation of China(Nos.81760625,81660576 and81560563)Projects of Guizhou Province(Nos.[2016]5623,JG[2016]06,[2019]1402,[2017]5609 and[2018]5781)。
文摘A quinine-derived thiourea-catalyzed inter-/intramolecular Michael cycloaddition of chromoneoxindole/benzofuranone synthons with 3-substituted methylenebenzofuranones has been established,which constructed enantiomerically pure bispiro[benzofuran-oxindole/benzofuran-chromanone]s bearing five consecutive stereocenters including two spiro quaternary carton centers in good yields(up to 93%) with high diastereoselectivities(up to>20:1 dr) and good enantioselectivities(up to>99% ee).Moreover,this is the first example of bifunctional chromone-benzofuranone synthon directed organocatalytic tandem reaction,and also the first example of the bispiro[benzofuran-oxindole] and bispirobenzofuranone,potentially useful in medicinal chemistry.
