氯化钴/邻菲罗啉催化氯苄双羰化合成苯丙酮酸的研究

双羰化是制备α-酮酸及其衍生物的重要反应 ,因其反应途径简捷且收率高而倍受青睐 ,国内外有不少关于氯苄双羰化合成苯丙酮酸的报道 .1 982年发现的钯配合物主要用于催化芳基卤代物的双羰化 [1] ;金子林等[2 ] 进行了八羰基二钴催化氯苄双羰化合成苯丙酮酸的研究 ,李光兴等[3 ] 近期也报道了吡啶 - 2 -羧酸钴的催化氯苄高效合成苯丙酮酸 .受前期吡啶 - 2 -羧酸钴催化双羰化研究成果的启发 ,我们进一步探讨了不同的席夫碱与氯化钴组成的催化体系的双羰化性能 .实验发现 ,采用“一锅煮”的方式 ,将氯化钴和邻菲罗啉 ( Phen)按一定比例加入到…     

在基础物理课程中开展数值计算的探索

阐述了在理、工科基础物理课程中进行数值计算的必要性和可行性；介绍了用Excel开展数值计算的方法和经验．     

（乙醇、异丙醇）+N-甲基哌嗪二元体系在101.3 kPa下的汽液平衡

采用改进的Rose釜测定乙醇 N-甲基哌嗪和异丙醇 N-甲基哌嗪两个二元体系在101.3kPa压力下的汽液平衡数据,用折光指数确定汽、液相组成,采用UNIQUAC活度系数模型关联实验数据,计算结果良好。     

公共交货期窗口的提前／延期惩罚

本讨论n个独立工件在一台机器上加工,而且加工时间服从正态分布的公共交货期窗口的提前/延期惩罚问题,在确定公共交货期窗口情况下,推导出工件的最优排序具有V型特征。     

超半球型浸没透镜在指纹图像采集中的应用

简要地叙述了指纹图像的应用意义。介绍了一台指纹采集装置 ,它主要由全反射棱镜、反射镜、双胶合透镜、超半球型浸没透镜、CCD等组成 ,并与计算机接口 ,从而实现了指纹采集过程的数字化 ,可以实时显示、存储指纹。着重地描述了超半球型浸没透镜的原理和成像特点。展示了几幅由指纹采集系统采集的指纹图像     

光栅摄谱仪的改进及其在周期性极化的铌酸锂晶体倍频研究中的应用

由于电荷耦合器件(CCD)具有光谱响应范围宽、检出限低、动态范围宽、暗电流和读出噪声低以及具有积分信号、多道同时检测和实时检测等能力的优点,在光谱测量和光谱成象领域获得了广泛的应用。将传统的1m光栅摄谱仪和科学CCD相结合,使其具有实时快速测量激光光谱的能力。将其应用于宽带双包层光纤激光在周期性极化的LiNbO₃晶体(PPLN)中倍频特性的研究,观察到了倍频激光光谱随PPLN控制温度的动态变化过程,并对此进行了详细分析。     

黄牛Sry基因5'端调控区序列研究

采用聚合酶链式反应(PCR)技术,以中国湖北雄性黄牛基因组DNA为模板,扩增出Sry基因5'端调控区680bp和640bp两个片段,并分别克隆到pUC18上,测序拼接出完整的5'调控序列1040bp,该序列含核心启动子和ATG起始密码.比较分析显示种内高度的进化保守性.这为Sry基因表达的时序控制、性别决定机制及进化等的深入研究奠定了基础.     

含硫杯[4]芳烃衍生物的合成及其紫外光谱研究

合成并表征了三个新的含硫且带醇羟基的杯「４」芳烃衍生物,核磁共振研究表明这些杯「４」芳烃都是Ｃｏｎｅ构型,对这些化合物的紫外光主普研究表明,在非极性溶剂中,在相对高浓度中,杯芳烃衍生物以形式存在。     

The chiral bioconversion and preclinical pharmacokinetic analysis of (R)‐(+)‐rabeprazole in beagle dogs by HPLC and HPLC‐MS/MS

In order to accurately investigate the preclinical pharmacokinetics of (R)‐(+)‐rabeprazole sodium injection, a reliable high‐performance liquid chromatography (HPLC) method was developed using a Chiral‐AGP column to prove that there is no chiral bioconversion of (R)‐(+)‐rabeprazole to (S)‐(?)‐rabeprazole in beagle dogs after single intravenous administration of (R)‐(+)‐rabeprazole sodium injection. An HPLC–tandem mass spectrometry (HPLC‐MS/MS) method for analysis of (R)‐(+)‐rabeprazole was developed and validated, and used to acquire the pharmacokinetic parameters in beagle dogs. (R)‐(+)‐Rabeprazole and internal standard omeprazole were extracted from plasma samples by protein precipitation and separated on a C₁₈ column using methanol–5 mm ammonium acetate as mobile phase. Detection was performed using a turbo‐spray ionization source and mass spectrometric positive multi‐reaction monitoring mode. The linear relationship was achieved in the range from 2.5 to 5000 ng/mL. The method also afforded satisfactory results in terms of sensitivity, specificity, precision, accuracy and recovery as well as the stability of the analyte under various conditions, and was successfully applied to a preclinical pharmacokinetic study in beagle dogs after single intravenous administrations of (R)‐(+)‐rabeprazole sodium injection at 0.33, 2 and 6 mg/kg. Copyright © 2013 John Wiley & Sons, Ltd.     

Regiospecific naphthyl nitration of 5,10,15,20‐tetranaphthylporphyrin

The nitration reaction of 5,10,15,20‐tetranaphthylporphyrin (TNP) was investigated in detail and the mono‐, di‐, and tri‐nitro‐TNPs were synthesized in high yield using 65% HNO₃. The ¹H‐NMR study shows that the preferred site of nitration of the naphthyl substituted porphyrin is the carbon atom of the meso‐substituents para to its bond to the porphyrin ring. The reaction leads to exquisite regioselectivity in favor of the mono, di, and tri‐nitro‐TNP. Quantum‐chemical ab initio calculations at different levels of theory were performed in order to explain the experimentally observed reactivity. Copyright © 2010 John Wiley & Sons, Ltd.