1-乙酰氨基-3,5-二甲基金刚烷的水解反应研究

通过对酰胺水解反应的机理的分析,针对1乙酰氨基3,5二甲基金刚烷空间位阻大、取代基为推电子基团的特点,对其水解反应对收率的影响进行了研究。结果表明:此化合物的水解适宜在碱性条件下进行,且在n(反应物)∶n(苛性钠)=1∶5,溶剂为水:乙二醇=1∶10,150℃下反应12h,得到最终产品盐酸美金刚的收率为92.5%,纯度为99.5%     

盐酸美金刚胺的合成及表征

通过比较不同的反应路线，确定了以1，3-二甲基金刚烷为原料，经溴代、乙酰氨基化、水解反应最后经酸化得到盐酸美金刚胺。改进并优化了合成路线，溴代反应确定为在回流条件下反应12h，n（1，3-二甲基金刚烷）：n（溴素）=1：1．5；水解反应条件是以，7（乙二醇）：n（水）=10：1为溶剂，150℃下反应12h，n（1-乙酰氨基-3，5-二甲基金刚烷）：n（氢氧化钠）=1：5，反应总收率达81．5％。产品用IR、ESI、^1HNMR、^13CNMR确证了产品的结构。     

环丙沙星在溶液中固液表面能的测定

采用激光法测定了环丙沙星在纯水和水－乙醇溶液（水体积分数23％）中的溶解度，介稳区和不同条件下的诱导期。根据经典成核理论和诱导期理论，推导了固液表面能与诱导期的理论关系，应用该理论关系计算了环丙沙星在溶液中的固液表面能，为环丙沙星初级成核与晶体生长研究提供了重要的参数。     

The reduction of l-cystine hydrochloride at stationary and rotating disc mercury electrodes

The kinetics of l-cystine hydrochloride reduction have been studied at a mercury-plated copper rotating disc electrode (RDE) and at a stationary mercury disc electrode (SMDE) in 0.1 mol dm⁻³ HCl at 298 K. The reduction of the disulphide is irreversible and hydrogen evolution is the major side reaction. In contrast to steady state electrode kinetic studies at a mercury drop electrode (which shows a well-defined limiting current), the mercury-plated Cu RDE shows overlap between disulphide reduction and hydrogen evolution. These effects are attributable to strong reactant adsorption with a calculated surface coverage close to 100%. A Tafel slope of −185 mV per decade is found with a cathodic transfer coefficient of 0.32 and a formal rate constant of 6.7 × 10⁻⁹ m s⁻¹. The relative merits of steady state voltammetry at a mercury-plated copper RDE and linear sweep voltammetry at the SMDE are discussed, as is the mechanism of l-cysteine hydrochloride formation.     

盐酸丁卡因的合成改进

以对氨基苯甲酸乙酯（苯佐卡因EPABA）为原料,经过N-烷基化、水解、酯化三步反应得到盐酸丁卡因粗品,产品收率 高达85.09%。采用FTIR、1HNMR和HPLC对产物进行了表征。对N-烷基化过程、水解条件、酯化条件进行了反应条件优化。结果表明：盐酸丁卡因被成功合成。N-烷基化的最佳工艺条件为：反应温度60℃, n（三乙胺）：n（EPABA）：n（1-溴丁烷）=1.2：1:4.6 ,合成对丁氨基苯甲酸乙酯（I）,产品收率为75.69%;与现有工艺路线相比,在生成关键中间体对丁氨基苯甲酸乙酯（I）时成功减少了双丁基化副产物的产生;水解反应的最佳合成条件为：原料配比为n(NaOH)∶n(对丁氨基苯甲酸乙酯)=1.4：1、反应温度为50℃、反应时间为8h, 合成对丁氨基苯甲酸（Ⅱ）,产品收率为99.78%;酯化反应的最佳反应条件为：原料配比为n〔（β-氯乙基）二甲胺盐酸盐〕： n(对丁氨基苯甲酸) =1.3：1、反应温度为116℃、溶剂为甲基异丁基甲酮,合成盐酸丁卡因,产品收率为85.09%。     

D-氨基葡萄糖盐酸盐的虾壳合成及其含量的紫外分光光度法测定

由预处理后的虾壳制备几丁质,以盐酸水解制得D-氨基葡萄糖盐酸盐,优化水解工艺,得到最佳工艺条件:水解盐酸浓度11.7mol/L,水解温度95℃,水解时间4h,收率63%,采用紫外分光光度法测定样品中D-氨基葡萄糖盐酸盐的含量为94.6%。     

Specific Ion Effects of Salt Solutions on Colloidal Properties of Octadecylamine Hydrochloride

Flotation continues to be a major technique for the production of potash from low grade, complex systems containing a variety of ores and ions. The specific ion effects on the behavior of the flotation collector in the KCl flotation system becomes important to the interpretation of the flotation mechanism. In this work, specific ion effects on the turbidity, surface tension and aggregation behavior of the common collector in KCl flotation, octadecylamine hydrochloride (ODA), have been investigated. The results from turbidity and surface tension studies of ODA solutions show that both cations and anions can affect the colloidal properties of ODA. Molecular dynamics simulations show that the binding that energy barrier between ODA headgroups and anions is principally responsible for the specific anion effect of γ _CAC of ODA solutions. In addition, the ion effect on the ODA aggregation particle size was also studied by using transmission electron micrographs (TEM) and dynamic light scattering. The data reveal that the presence of salt ions can induce the formation of larger ODA colloidal particles, on which the cation effect is more significant. This work provides detailed information of specific ion effect on colloidal properties of ODA, which may promote a further understanding of the flotation mechanism and help to improve the flotation of KCl from brine sources.     

离子色谱法测定灭多威中的盐酸羟胺

建立了离子色谱-柱后衍生测定灭多威中痕量盐酸羟胺的新方法。样品经净化后,采用Ion Pac CS16离子交换色谱柱、安培检测器检测,外标法定量。结果表明:盐酸羟胺在0.02~1.0 mg/L质量浓度范围内,线性关系良好,线性相关系数为0.999 8。方法回收率为95.3%~98.1%,相对标准偏差均小于3%。检出限(信噪比3)为2.5μg/L。该方法简便,灵敏度高,无杂质干扰,前处理简便,可用于灭多威中痕量盐酸羟胺的测定。     

Solubility and Apparent Specific Volume of Some Pharmaceutical Salts in Propylene Glycol + Water Mixtures at 298.15 K

The equilibrium solubility of three pharmaceutical salts, namely, sodium naproxen (Na.NAP), procaine hydrochloride (PC.HCl), and lysine clonixinate (Lys.Clon), was determined in propylene glycol (PG) + water mixtures at 298.15 K. If the mole fraction concentration scale is considered, the mixtures’ composition-dependence on solubility was different for these drugs. Thus, the solubility of Na.NAP increased nonlinearly from pure water to pure PG. By contrast, the solubility of PC.HCl decreased nonlinearly from pure water to pure PG. In a different way, the solubility of Lys.Clon increased from pure water to the mixture with mass fraction of PG, w₁ = 0.80, and later, it decreased to reach a lower value in pure PG. A good correlation of the solubility data was obtained by using the modified NIBS/R-K model. Otherwise, the apparent specific volumes at saturation of these drugs were also calculated in all the mixtures under study.