（S）-噻吗洛尔半水合物的合成及表征

为了开发β受体阻断剂新药（S）-噻吗洛尔半水合物，采用3-吗啉-4-氯-1，2，5-噻二唑为起始原料，经水解反应得到中间体1（3-吗啉-4-羟基-1，2，5-噻二唑）。中间体1与R-环氧氯丙烷发生醚化反应，经后处理及重结晶得到中间体2 {（R）-4-［4-（环氧乙烷-2-基甲氧基）-1，2，5-噻二唑-3-基］吗啉}。中间体2经胺化反应、马来酸成盐及重结晶得到（S）-马来酸噻吗洛尔。（S）-马来酸噻吗洛尔经游离、纯水转晶得到符合药典标准的（S）-噻吗洛尔半水合物，总收率14.05%且e.e.值为99.66%。最终成品经IR、1H-NMR、13C-NMR、MS、TGA、DSC表征，并优化各步反应条件。结果表明:以三乙胺为醚化反应缚酸剂75 ℃反应最佳；以乙醇为胺化反应溶剂46 ℃反应16 h最佳；S-噻吗洛尔的转晶拆分以水作溶剂，比传统不对称合成工艺安全稳定，操作简单，适合工业化生产。     

Isolated hepatic tuberculosis mimicking liver tumors in a dialysis patient

Cases of isolated hepatic tuberculosis (TB) are rare. The diagnosis is often delayed or missed because of nonspecific symptoms and laboratory findings. Besides, the disease is extremely rare even in a country where TB is an alarming public health problem. This report demonstrates the difficulty in correctly diagnosing local hepatic TB. We report the case of a 62‐year‐old male patient with end‐stage renal disease treated with hemodialysis, who developed 2 months of abdominal distension and general anorexia, with hyperechoic hepatic lesions on ultrasound. Computed tomography suspected multiple liver tumors. The liver biopsy finally led to the diagnosis of TB of the liver without other involvements. We conclude that isolated hepatic TB is one of the rare forms of extrapulmonary TB in dialysis patients. A greater awareness of this rare clinical entity may prevent needless surgical interventions.     

Facile synthesis of Li 2 ZrO 3 -modified LiNi 0.5 Mn 0.5 O 2 cathode material from a mechanical milling route for lithium-ion batteries

Li2ZrO3-modified LiNi0.5Mn0.5O2 materials with improved electrochemical performance were directly synthesized by a simple mechanical milling route with ZrO2, Li2CO3 and Ni0.5Mn0.5(OH)2 precursors...     

Ca-Mg-Al复合氧化物催化尿素与1,2-丙二醇制碳酸丙烯酯

采用共沉淀法制备了系列Ca-Mg-Al复合氧化物催化剂，通过对沉淀剂配比、沉淀液pH值及焙烧温度等制备条件的考察，得到以Na₂CO₃为沉淀剂、pH=9.5、850℃下焙烧4h制备的Ca-Mg-Al催化活性最高。在 n(PG)∶n(urea)=1.5∶1、反应温度为145℃、绝压20kPa、反应时间4h、催化剂用量为尿素质量的5%时，碳酸丙烯酯收率达到84.6%。采用XRF、XRD、NH₃-TPD、SEM及BET对催化剂的组成、晶型及酸性进行了表征，发现随着沉淀剂中Na₂CO₃的含量增加，催化剂中CaO∶MgO的比例增大，碳酸丙烯酯的收率亦升高；经850℃焙烧后，催化剂中存在CaO和MgO两种活性中心，起协同催化作用；随着焙烧温度由700℃升高到850℃，NH₃-TPD脱附曲线向低温方向偏移，且强酸中心NH₃脱附峰面积比由81.14%明显下降为0，中强酸中心NH₃脱附峰面积比由0增加到78.07%，而碳酸丙烯酯收率由68%增加到84.6%，这表明催化剂强酸性位的减少是催化活性增加的主要原因。     

Unusual Two-Step Assembly of a Minimalistic Dipeptide-Based Functional Hypergelator

Self-assembled peptide hydrogels represent the realization of peptide nanotechnology into biomedical products. There is a continuous quest to identify the simplest building blocks and optimize their critical gelation concentration (CGC). Herein, a minimalistic, de novo dipeptide, Fmoc-Lys(Fmoc)-Asp, as an hydrogelator with the lowest CGC ever reported, almost fourfold lower as compared to that of a large hexadecapeptide previously described, is reported. The dipeptide self-assembles through an unusual and unprecedented two-step process as elucidated by solid-state NMR and molecular dynamics simulation. The hydrogel is cytocompatible and supports 2D/3D cell growth. Conductive composite gels composed of Fmoc-Lys(Fmoc)-Asp and a conductive polymer exhibit excellent DNA binding. Fmoc-Lys(Fmoc)-Asp exhibits the lowest CGC and highest mechanical properties when compared to a library of dipeptide analogues, thus validating the uniqueness of the molecular design which confers useful properties for various potential applications.