An efficient synthesis of δ-glyconolactams by intramolecular Schmidt–Boyer reaction under microwave radiation

δ-Glyconolactams were first synthesized by the intramolecular Schmidt–Boyer reaction using corresponding δ-azidosugars as starting material. The reaction could be efficiently performed in good yields of 61–69% under microwave radiation in acid condition, providing an alternative protocol to iminosugar δ-lactam.     

Triphenylamine derivatized phenylacetylene macrocycle with large two-photon absorption cross-section

A phenylacetylene macrocycle (PAM) derivative containing triphenylamine as the framework was synthesized in one-step Sonogashira coupling. The photophysical and electrochemical properties were investigated in details. This hexamer shows significant enhancement in two-photon absorption cross-section relative to reported PAM derivatives.     

UPLC-ELSD Determination of 1-Octacosanol in Raw Material and Health Products

Determination of the levels of 1-octacosanol is important in food stuff for the study of its pharmacological activities and health benefits. In this study, a novel, simple and fast internal standard method for the non-derivatization ultra-performance liquid chromatographic determination of 1-octacosanol in raw materials and health products was developed and validated based on evaporative light scattering detection. The linearity (r ² > 0.998), recovery (99.1–100.2%, RSD <2.7%), intra- and inter-day precision (RSD <3.8%), limit of detection (1.0 mg/L), limit of quantification (2.2 mg/L) of the 1-octacosanol were determined. The method was successfully applied to nine real 1-octacosanol products. The results of analyses had close agreement with the labeled claims of 1-octacosanol content in these products. Compared with the classical gas chromatography method, the developed method was simpler, faster and more environmentally friendly due to avoiding any derivatization step. This protocol represents a rapid and feasible method for quality control of 1-octacosanol products.

     

Organophosphine/phosphite‐stabilized silver(I) complexes bearing N‐acetylbenzamide ligand: synthesis,characterization and potential application in metal organic chemical vapor deposition

New N‐silver(I) acetylbenzamide complexes of type L_n?AgNC₉H₈O₂ (L = PPh₃; n = 1, 2a; n = 2, 2b; n = 3, 2c; L = P(OEt)₃; n = 1, 2d; n = 2, 2e; n = 3, 2f) were prepared. These complexes were obtained in high yields and characterized by elemental analysis, ¹H NMR, ¹³C{H} NMR, ³¹P{H} NMR and IR spectroscopy, respectively. The molecular structure of 2b has been determined by X‐ray single‐crystal analysis in which the silver atom is in a distorted tetrahedral geometry and crystallizes as cis–trans. New N‐silver(I) acetylbenzamide complexes have a four‐membered ring, which could influence their chemical and physical properties and modulate volatility. Metal organic chemical vapor deposition experiments were carried out successfully at 400°C and 450°C using 2e as precursor for the deposition of silver films, respectively. The high‐purity silver film obtained at 400°C is dense and homogeneous. Copyright © 2012 John Wiley & Sons, Ltd.     

Copper‐catalyzed Clauson–Kass pyrroles synthesis in aqueous media

An efficient and convenient copper‐catalyzed Clauson–Kass reaction of 2,5‐dimethoxytetrahydrofuran with amines in aqueous media has been developed, providing a wide range of N‐substituted pyrroles in good yields. It is noteworthy that the Clauson–Kass reaction of 2,5‐dimethoxytetrahydrofuran with p‐phenylenediamine or m‐phenylenediamine proceeds smoothly to afford the corresponding monopyrroles and bispyrroles with high selectivity in impressive yields. A plausible mechanism for the formation of N‐substituted pyrroles has been proposed. Copyright © 2012 John Wiley & Sons, Ltd.     

银胶体系中吖啶橙、吡啶共吸附竞争的研究

本文利用光学多道分析仪,着重研究了吖啶橙—银胶—吡啶体系;观察了吖啶橙荧光的两次瞬间增强的时间效应荧光谱;分析了吖啶橙与吡啶在银表面上共吸附竞争以及氯化钾在这一竞争中所起的作用。对于表面与分子间相互作用的这一规律作了初步探讨。     

氧络双四苯骈卟啉铁（Ⅲ）的合成及氧络二聚反应的热力学研究

合成了氧络双四苯骈卟啉铁（Ⅲ），其结构经红外光谱、紫外光谱和元素分析确证．同时用分光光度法研究了在ＤＭＦ－Ｈ２Ｏ体系中四苯骈卟啉铁（Ⅲ）的氧络二聚反应的热力学平衡，并由此计算出该反应的有关热力学常数．