通过两种不同的合成途径合成了在环状咪唑并[1,2- a ] [1,8]萘吡啶基介电卡宾骨架上带有质子响应性羟基单元的Cp * Ir(III)配合物(1)。的分子结构1揭示了配体的阴离子内酰胺形式。通过1 H NMR和UV-vis光谱检查了配体支架上内酰胺-内酯互变异构体之间的酸碱平衡。估算内酰胺形式为1的附件-OH基团的p K a,以评估催化剂的质子转移性能。1的催化功效通过使用三种不同的氢源(分子H 2,i PrOH / KO t Bu组合和HCOOH / Et 3 N(5:2)共沸混合物)评估醛的还原胺化反应。发现在三种不同的氢化方法中,HCOOH / Et 3 N(5:2)共沸混合物是最好的。在反应条件下,催化剂1在羰基上化学选择性地氢化亚胺。使用HCOOH / Et 3 N(5:2)共沸混合物将一系列醛还原为相应的仲胺。此外,催化剂1在还原多种N-杂环亚胺衍生物方面显示出高效率。提
Sequential hydroaminomethylation/Pd-catalyzed hydrogenolysis as an atom efficient route to valuable primary and secondary amines
作者:Jacquin October、Selwyn F. Mapolie
DOI:10.1016/j.tetlet.2021.153018
日期:2021.4
valuable primary and secondary amines is reported using a sequential procedure of hydroaminomethylation and Pd-catalyzed hydrogenolysis. The hydroaminomethylation reaction was catalyzed by a cationic Rh(I) iminopyridyl complex and the N-alkylated benzylamines were produced with high chemoselectivity, albeit as mixtures of linear and branched products. Performing the hydrogenolysis reaction using 10% Pd/C
Materials for hydrophilic interaction chromatography and processes for preparation and use thereof for analysis of glycoproteins and glycopeptides
申请人:Waters Technologies Corporation
公开号:US10119944B2
公开(公告)日:2018-11-06
The invention relates to poly-amide bonded hydrophilic interaction chromatography (HILIC) stationary phases and novel HILIC methods for use in the characterization of large biological molecules modified with polar groups, known to those skilled in the art as glycans. The invention particularly provides novel, poly-amide bonded materials designed for efficient separation of large biomolecules, e.g. materials having a large percentage of larger pores (i.e. wide pores). Furthermore, the invention advantageously provides novel HILIC methods that can be used in combination with the stationary phase materials described herein to effectively separate protein and peptide glycoforms by eliminating previously unsolved problems, such as on-column aggregation of protein samples, low sensitivity of chromatographic detection of the glycan moieties, and low resolution of peaks due to restricted pore diffusion and long intra/inter-particle diffusion distances.
Porous materials for solid phase extraction and chromatography and processes for preparation and use thereof
申请人:Brousmiche Darryl W.
公开号:US10258979B2
公开(公告)日:2019-04-16
The invention provides novel porous materials that are useful in chromatographic processes, e.g., solid phase extraction, and that provide a number of advantages. Such advantages include superior wetting characteristics, selective capture of analytes of interest, and non-retention of interfering analytes. In certain aspects, the materials feature at least one hydrophobic component, at least one hydrophilic component and a average pore diameter of about 100 Åto about 1000 Å. In certain embodiments the materials also exhibit a nitrogen content from about 1% N to about 20% N. In certain embodiments, the materials also exhibit more than 10% of the BJH surface area of the porous material is contributed by pores that have a diameter greater than or equal to 200 Å. The invention advantageously provides novel porous materials having a large percentage of larger pores (i.e. wide pores). The invention advantageously provides novel porous materials that overcome the problems of SPE of biological samples.
本发明提供的新型多孔材料可用于色谱过程,如固相萃取,并具有许多优点。这些优点包括优异的润湿特性、选择性捕获感兴趣的分析物以及不截留干扰分析物。在某些方面,这些材料具有至少一种疏水成分、至少一种亲水成分和约 100 Å 至约 1000 Å 的平均孔径。在某些实施例中,材料的氮含量从约 1% N 到约 20% N。在某些实施例中,材料还显示多孔材料 10% 以上的 BJH 表面积是由直径大于或等于 200 Å 的孔贡献的。本发明提供的新型多孔材料具有很大比例的较大孔隙(即宽孔隙)。本发明提供的新型多孔材料克服了生物样品 SPE 的问题。
MONOLITHIC ELECTROKINETIC PUMP FABRICATION
申请人:Waters Technologies Corporation
公开号:EP2079665A2
公开(公告)日:2009-07-22
POROUS MATERIALS FOR SOLID PHASE EXTRACTION AND CHROMATOGRAPHY