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991.
Ling Yan Liang Qiao Ji Ji Yixin Li Xuefei Yin Ling Lin Xiaohui Liu Jun Yao Yi Wang Bin Liu Kun Qian Baohong Liu Pengyuan Yang 《Analytica chimica acta》2017
Mass spectrometry (MS)-based proteome profiling is essential for molecular diagnostics in modern biomedical study. To date, sample preparation including protein extraction and proteolysis is still very challenging and lack of efficiency. Recently tips-based sample preparation protocols exhibit strong potentials to achieve the goal of “a proteome in an hour”. However, in-tip proteolysis is still rarely reported and far from ideal for dealing with complex bio-samples. In this work, nanoreactors encapsulated micropipette tips were demonstrated as high performance devices for fast (∼minutes) and multiplexing proteolysis to assist the profiling of cancer cells proteome. Nanoporous silica materials with controlled pore size and surface chemistry were prepared as nanoreactors and encapsulated in micropipette tips for efficient in situ proteolysis. The as-constructed device showed desirable sensitivity (LOD of 0.204 ± 0.008 ng/μL and LOQ of 0.937 ± 0.055 ng/μL), selectivity, stability (two months under −20 °C), reusability (at least 10 times), and little memory effect in MS based bottom-up proteomic analysis. It was used for comprehensive protein mapping from cancer cell lines. The number of identified proteins was increased by 18%, 22%, 52%, and 52% dealing with HepG2, F56, MCF7, and HCCLM3 cancer cells, compared to traditional in-solution proteolysis based bottom-up proteomic strategy. With the enhanced performance, our work built a novel, efficient and miniaturized platform for facile proteomic sample preparation, which is promising for advanced biomarkers discovery in biomedical study. 相似文献
992.
Xiaolong Wan Jiadong Hu Dongyang Xu Yang Shang Yanxia Zhen Chenchen Hu Fan Xiao Yu-Peng He Yisheng Lai Weiqing Xie 《Tetrahedron letters》2017,58(12):1090-1093
A Re2O7 catalyzed cycloetherification of monoallylic diols is described. The reaction features short reaction time, mild reaction conditions and exclusive E selectivity. A wide range of monoallylic alcohols with alkyl or aryl substituents on olefin smoothly undergo ring closure to deliver corresponding oxa-heterocycles. The reaction is also operationally simple and not sensitive to air and moisture. 相似文献
993.
A novel tandem one-pot method for the synthesis of polysubstituted pyridine derivatives has been developed via Knoevenagel-type reaction and subsequent 6π electrocyclization of the Blaise reaction intermediates and 3-formylchromones. Short reaction time, moderate to good yields and excellent functional group tolerance have been accomplished in this protocol. 相似文献
994.
Xue-Min Tan Qiao-Mei Lai Zhi-Wei Yang Xiao Long Hai-Lin Zhou Xiao-Lin You Xiao-Jie Jiang Hai-Lei Cui 《Tetrahedron letters》2017,58(2):163-167
A La(OTf)3 catalyzed synthesis of tetrasubstituted pyrroles under microwave irradiation has been developed affording various α-aryl tetrasubstituted pyrroles in acceptable to good yields (36–82% yield) through condensation/alkyne azacyclization/isomerization sequence. Functionalized α-aryl pentasubstituted pyrroles could be prepared from tetrasubstituted pyrroles through easy transformations. 相似文献
995.
A practical copper-catalyzed N-arylation of NH-containing heterocycles with arenediazonium tetrafluoroborates has been developed using CuCl as catalyst and K2CO3 as additive under ligand-free conditions. This reaction system has wide substrate scope including imides, 1H-pyrazole, 1H-tetrazoles, 1,2-benzisothiazol-3(2H)-one, and related sulfonamides and gives moderate to excellent yields (up to 95%) of the desired products. This strategy is very general, simple, environmentally friendly, and tolerant of oxygen. 相似文献
996.
Sheng-Rong Liao Yong Tang Liang Xu Xue-Feng Zhou Jun-Feng Wang Bin Yang Yong-Hong Liu 《Tetrahedron》2017,73(1):98-107
An unexpected ring-contraction from benzo[b]pyrazino[1,2-d][1,4]thiazine-1,4-diones (6) to benzo[4,5]thiazolo[3,2-a]pyrazine-1,4-diones (7) has been developed. The preliminary mechanistic studies showed the transformation contained two independent steps: the first step is the formation of a Michael adduct upon the addition of the protic solvent, in the presence of base, to the C-2-C-3 double bond of compound 6, and the second step is a ring-contraction induced by oxygen via the migration of sulfur atom from C-2 to C-3 position. And its scope is also studied. 相似文献
997.
A new strategy for the C(sp2)–H imidation and 1,2-imidofluorination of vinylsulfides has been established through simple treatment with N-fluorobis(benzenesulfonyl)imide, which acts as both oxidant and nitrogen source. For alkyl and electron-rich aryl vinylsulfides, alkyl/arylthioenamines are produced in up to 92% total yields. However, for steric and electron-deficient aryl vinylsulfides, 1,2-imidofluorination products are prepared in up to 73% yields. The chemoselectivity is controlled by the steric and electronic effects of aryl substituents. Thionium ions are proposed as key intermediates in the two reactions. 相似文献
998.
Triphenylphosphine-mediated metal-free trifluoromethylthiolation and difluoromethylthiolation of thiols by CF3SO2Cl and CHF2SO2Cl to synthesize trifluoromethyl disulfides and difluoromethyl disulfides, respectively, was achieved at room temperature. Iodine generated in situ from iodide facilitated this reaction via the formation of iodotriphenylphosphonium iodide which could serve as a reducing agent in this transformation. Readily available reagents and mild reaction conditions without transition-metals allow this protocol to be more practical than traditional methods. 相似文献
999.
Qin Yang Miao-Miao Liang Hui-Jun Wang Qi-Qi Zhao Hua-Jie Zhu Li Liu Charles U. Pittman 《Tetrahedron》2017,73(17):2432-2438
The experimental optical rotation (OR), electronic circular dichroism (ECD) and vibrational circular dichroism (VCD) spectra of (R)-3-hydroxy-4,5-dimethylfuran-2(5H)-one (sotolon, 1) and (R)-5-ethyl-3-hydroxy-4-methylfuran-2(5H)-one (maple furanone, 2) taken in chloroform were compared to their spectra calculated with time-dependent density functional theory (TDDFT). Sotolon was shown to exist as a dimer in chloroform while maple furanone remains a monomer. Transition state barriers for the enol/keto tautomerization of sotolon were calculated and found to be high. The VCD method offers promise to ultimately distinguish between the presence of monomers or dimers. 相似文献
1000.
Qing-Dong Wang Jin-Ming Yang Dong Fang Jiangmeng Ren Bu-Bing Zeng 《Tetrahedron letters》2017,58(30):2877-2880
An efficient iodine-catalyzed chemoselective 3-formylation of free (N–H) and N-substituted indoles was achieved by using hexamethylenetetramine (HMTA) in the presence of activated carbon under air atmosphere. This new method could provide 3-formylindoles in moderate to excellent yields with fairly short reaction times. Moreover, this catalytic formylation of indoles procedure can be applied to gram-scale synthesis. 相似文献