Synthesis and Crystal Structure of N3-（Dimethyl- pyrimidine）-N4-（tri-O-acetyl-xylosyl） Thiourea

The crystal structure of the title compound （C18H24N4O7S, Mr = 440.47） was prepared by the condensation of 2,3,4-tri-O-acetyl-β-D-xylopyranosyl isothiocyanate with 4,6-dimethylpyrimidin-2-amine and structurally determined by single-crystal X-ray diffraction. The crystal belongs to the monochnic system, space group P2 1 with a = 7.5500（17）, b = 10.498（2）, c = 14.208（3） A, β = 99.929（4）°, V = 1109.2（4） A^3, Z = 2, Dc = 1.319 g/cm^3,μ = 0.191, F（000） = 464, Flack = 0.00（15）, R = 0.0684 and wR = 0.1103. In the crystal structure, the xylose ring adopts a ^4C1 chair conformation. Due to the hydrogen bonding interaction between N（4）-H（4A） and N（1）, the pyrimidine ring is well positioned.     

Common methods for the chiral determination of amphetamine and related compounds I. Gas, liquid and thin-layer chromatography

This article reviews the most common, useful methods for the chiral determination of amphetamine (AM) and AM-derived designer drugs in different of matrix, including blood, hair, urine, medicaments or standard solutions, taking into consideration articles published in the past 15 years. We consider chromatographic methods (e.g., gas, liquid, high-performance liquid, and thin layer). We describe several types of chiral derivatization reagent, mobile-phase additive and chiral stationary phase commonly used in the chromatographic methods. Tables summarize basic information about conditions (e.g., type of column and mobile phase), detection mode and reference data for each procedure.     

纳米银对表面吸附荧光素的荧光增强和荧光猝灭效应及KCl的荧光猝灭释放效应

制备了两种不同粒径的纳米银溶胶，研究了在水溶液条件下其对表面吸附荧光素(FL)的荧光性能的影响及KCl电解质对该体系荧光性能的影响。FL溶液中加入纳米银，FL分子吸收峰位发生红移。随着纳米银浓度的增加，FL分子荧光先出现增强，而后又逐渐猝灭。粒径较大的纳米银产生最大荧光增强比率所需浓度较低。在纳米银猝灭FL分子荧光的溶液中加入KCl电解质，随着KCl浓度的增加，荧光逐渐增强，出现了荧光猝灭释放效应。研究结果表明，纳米银对表面吸附FL的荧光作用与FL分子附近局域电磁场增强和分子到金属表面无辐射跃迁能量转移过程决定并与纳米银的浓度、尺寸及电解质等密切相关。     

稀土-荧光素双重荧光响应pH探针分子的合成与荧光性质研究

将含有8-氨基喹啉与荧光素衍生物缩合的席夫碱QZ1与铕髥的TTA(噻吩基三氟乙酰丙酮)化合物作为基本原料合成了新的铕髥-荧光素化合物Eu-QZ1,并对其进行了光谱表征。化合物Eu-QZ1在470 nm光的激发下产生荧光素的特征绿色荧光(530 nm)。在从碱到酸(pH从9.0到6.0)滴定过程中该荧光的强度增强了接近5倍,其pKa值计算为7.30。在370 nm光的激发下,Eu-QZ1发射稀土铕髥离子的特征红色荧光(主峰位于612 nm)。在从酸到碱(pH从5.5到8.5)滴定过程中,该荧光的强度增强了接近10倍,其pKa值计算为7.39。这些结果表明Eu-QZ1是1个高灵敏度双荧光响应的pH探针。细胞试验表明Eu-QZ1具有良好的细胞通透性,能够在红光和绿光两个位置标记海拉细胞中的pH范围。     

以TritonX-100为增敏剂荧光速率法测定银

基于醋酸钠介质中，银（Ⅰ）催化过硫酸钾氧化荧光素反应，以２，２－联吡啶为活化剂，Ｔｒｉｔｏｎ Ｘ－１００为增敏剂，拟定了测定痕量银的新荧光速率法。本法由于添加 Ｔｒｉｔｏｎ Ｘ－１００表面活性剂，使得灵敏度提高了４倍，测定银含量线性范围为２～３２ μｇ／Ｌ，相对标准偏差为３．１％（ｎ＝９），检出限为１．７６ × １０－３（ｍｇ／Ｌ）。用于测定氯化银的溶度积和光谱感光板中的银，结果满意。     

Synthesis and mesomorphic behaviour of high polarisability materials for non-linear optical applications

A variety of high polarisability materials have been synthesised with thioester and alkyne linking groups, and isothiocyanato and cyano terminal groups. The synthesis of these materials is presented and the transition temperatures and optical parameters of the materials are discussed and compared to those of the parent ester and non-linked analogues. The thioester and isothiocyanate units provide very high polarisabilities although the isothiocyanato unit leads to reduced mesophase thermal stabilities when compared to analogous cyano-terminated mesogens.     

反相高效液相色谱测定依替巴肽注射液中氨基酸的含量

采用异硫氰酸苯酯为柱前衍生化试剂,结合反相高效液相色谱技术,建立了定量分析依替巴肽注射液中氨基酸组分的检测方法。优化色谱条件,选用Agilent XDB-C18色谱柱(5μm,150 mm×4.6 mm),以0.1 mol/L醋酸钠(冰醋酸调至pH 6.0)-乙腈(90∶10)为流动相A,乙腈为流动相B,梯度洗脱方式,检测波长为254 nm,流速为1.0 mL/min,进样体积为5μL,柱温为30℃。结果表明,在优化条件下,各氨基酸能实现有效分离,且在1.23～3.68 mmol/L浓度范围内,各氨基酸的线性关系良好,相关系数(r)为0.999 1～0.999 6。该方法显示了良好的准确性、重复性、稳定性及选择性,能对依替巴肽注射液中的氨基酸实现准确定量分析。     

A Convenient Synthesis of 1-Amino-4-methyl-4H-3-thia-4,5a,10-triazacyclopenta[a]fluoren-5-ones and Some New 2,3-Dihydro-1,3,4-thiadiazoles

1-amino-4-methyl-4H-3-thia-4,5a,10-triazacyclopenta-[a]fluoren-5-one and 6-methyl-6H-,9H-thia-4b,6,9,11,12-pentaazaindeno[1,2-a]-fluorene-5,8-dione derivatives were prepared from 2-methyl-1-oxo-3-thioxo-2,4,9b-trihydropyrimidino[1,6-a] benzimidazole-4-carbonitrile. Also, 2,3-dihydro-1,3,4-thidazoles were synthesized via a reaction of hydrazonoyl chlorides with 3-(methylamino)-2-substituted 3-thioxopropanenitrile. Structures of newly synthesized compounds were elucidated on the basis of elemental analyses, spectral data, and alternative methods synthesis whenever possible.     

分光光度法测定钻井液中示踪剂荧光素钠

研究了钻井液示踪剂荧光素钠的分光光度法测定方法。在pH9.0的乙酸钠缓冲介质中,用5cm比色皿于波长485nm条件下,分光光度法测定钻井水示踪剂荧光素钠的测量下限为0.005μg/mL。对荧光素钠含量为0.012μg/mL的水样,测量相对标准偏差(RSD)为8.7%,可以满足钻井水示踪技术要求。     

Efficient Preparation of Isothiocyanates From Dithiocarbamates Using Bromineless Brominating Reagent

For the first time, the crystal structure of a ditribromide reagent 1,1′-(ethane-1,2-diyl)dipyridinium bistribromide (EDPBT) has been determined. Utilizing this thiophilic bromineless brominating agent EDPBT, highly useful synthetic intermediates (alkyl and aryl isothiocyanates) have been achieved directly from dithiocarbamates. EDPBT can be easily prepared from readily available reagents. It has been used as a thiophilic reagent, and its thiophilicity dominates over its brominating ability for substrates amenable to bromination. This is a sustainable process for the preparation of isothiocyantes because the spent reagent can be recovered, regenerated, and reused.