紫外光谱法检测水中咪唑类离子液体的含量

介绍了用紫外光谱测定水中离子液体含量的方法。测定了7种离子液体([C4mim][Cl]、[C4mim][BF4]、[C4mim][PF6]、[C5mim][Cl]、[C6mim][BF4]、[C8mim][Cl]和[C8mim][BF4])的最大吸收波长,并且绘制了校准曲线。结果表明,在实验试剂用量范围内,离子液体在波长211nm附近的吸光度与浓度呈线性关系,其线性相关系数均大于0.999。说明用紫外光谱法检测水中离子液体含量简单、快速且测定结果准确可靠。     

4,4,5,5-四甲基-1,3,2-二氧硼戊环的11B NMR及1H-11B HMQC研究

以4,4,5,5-四甲基-1,3,2-二氧硼戌环分子为研究对象,对碳硼烷类化合物的核磁共振(NMR)检测方法进行了研究.除了采用常规的核磁共振碳谱(~(13)C NMR)、氢谱(~1H NMR)及其二维相关谱外,引入核磁共振硼谱(~(11)B NMR)与二维异核多量子相关谱(~1H-~(11)B HMQC),对含硼类化合物结构进行了测定,该方法对于准确解析硼烷类化合物的结构具有较好的参考意义.     

1,5-二芳基-3-氯甲基硫代-1H-1,2,4-三唑的合成及其结构表征

1-芳酰基-3-苯氨基硫脲与二氯甲烷在无溶剂条件下反应合成了4种1,5-二芳基-3-氯甲基硫代-1H-1,2,4-三唑类化合物,产率为64%-74%.产物的结构通过红外光谱、核磁共振光谱和高分辨质谱进行了表征.     

系列甲基苯基卟啉-5-氟尿嘧啶化合物的合成与表征

设计合成了6种甲基苯基卟啉-5-氟尿嘧啶化合物。通过红外光谱、紫外-可见光谱、核磁共振谱和质谱对所合成的化合物结构进行了确认。探索出了合成反应的最佳条件和目标化合物的分离纯化方法。实验结果表明,选择DMF为溶剂,反应温度在115℃,反应时间2h,产率较高,A1、A2,B1、B2、C1和C2分别为25.66%、25.02%,24.89%、26.17%、28.43%和24.19%;采用硅胶G(粒径为48—75μm)柱层析,分离效果较好。     

具有潜在抗菌活性的环丙沙星衍生物的NMR谱研究

利用核磁共振谱,通过¹H-¹]H COSY, gHMBC and APT (Attached Proton Test)实验对所合成的新化合物1环丙基-6-氟-7-（4-苯乙酰氨基硫代甲酰基-1-哌嗪基）-1,4-二氢-4-氧代喹啉-3-羧酸的NMR谱进行了分析,并对其谱峰进行了详细归属.     

新型吡唑并[3,4-d]嘧啶-4-酮类衍生物的结构表征和镇痛活性

本文以2-氰基-3-乙氧基丙烯酸乙酯与3,4-二甲基苯肼为原料,通过多步反应合成了三种新型吡唑并[3,4-d]嘧啶-4-酮类衍生物（A~C）,通过核磁共振（NMR,包括¹H NMR、¹³C NMR）和液相色谱-质谱联用（LC-MS）技术表征确证了其结构,并完整归属了三种化合物的¹H NMR数据．对所合成的化合物1-(3,4-二甲基苯基)-6-甲基-5-[3-(哌啶-1-基)丙氧基]-1,5-二氢-4H-吡唑并[3,4-d]嘧啶-4-酮（A）,通过小鼠脑部质谱成像和福尔马林实验进行了初步的体内镇痛活性评价,我们发现化合物A能透过血脑屏障,并产生显著且剂量依赖的镇痛活性．本研究为以吡唑并[3,4-d]嘧啶-4-酮为骨架的镇痛药物的研发提供了结构和体内活性的基础研究数据．     

手性γ-内酰胺类化合物立体化学的研究

采用向关键中间体7a-(2, 4-二氯苯基)-3-苯基-2, 3, 4, 6, 7, 7a-六氢-５H-吡咯并[2, 1-b]- 唑-5-酮（化合物1）引入一个已知手性中心的策略,通过2D 1H-1H COSY谱和1D NOESY谱对化合物1和手性化合物α-[(2-甲基-3-氯苄基）氨甲酰基甲基]-γ-(2, 4-二氯苯-基)-N-{[3-(哌啶-1-基)丙基]氨甲酰基甲基}-γ-内酰胺（化合物2)的立体化学进行了研究．该方法对这类手性γ-内酰胺类化合物绝对构型的确定具有准确、方便、简单、快捷的特点．     

2-甲基-6-(2-甲苯基)-2-庚烯的波谱学研究

采用色谱法从蒲儿根花部位中分离得到2-甲基-6-(2-甲苯基)-2-庚烯,该化合物第一次以单体的形式得到,通过测定氢-氢相关谱(1H-1H COSY)、DEPT谱、异核单量子相关谱(HSQC)及异核多键相关谱(HMBC)等二维谱确定了该化合物的结构,并对该化合物的1H NMR和13C NMR谱进行了归属.     

TRANILAST ^1H^13CNMR谱分析及其结构的鉴定

本文用COSY,CHCOR等二维核磁共振技术对TRANILAST,2[]3-(3.4-二甲基苯基)1-氧代-2-丙烯基]氨基]苯甲到进行了~1H、~(13)C NMR谱数据分析及归属,并结合~(13)C弛豫时间T_1 及变温实验对合成产品进行了结构鉴定.     

2,4-二取代-1,3,4-噻二唑衍生物的合成与结构表征

1-芳酰基-3-苯氨基硫脲与二氯甲烷在无溶剂条件下反应合成了2种2,4-二取代-1,3,4-噻二唑类化合物,产率为50％-70％.产物的结构通过红外光谱、核磁共振光谱和高分辨质谱进行了表征.     

Volumetric, acoustic and spectroscopic studies for binary mixtures of ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) with alkoxyalkanols at T = (288.15 to 318.15) K

Densities and speeds of sound have been measured for the binary mixtures of ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate [bmim][PF₆] with ethylene glycol monoethyl ether (EGMEE), diethylene glycol monoethyl ether (Di-EGMEE), triethylene glycol monoethyl ether (Tri-EGMEE) over the whole composition range at atmospheric pressure. Experimental densities have been used to estimate excess molar volumes, V^E. Changes in isentropic compressibility, Δκ_s have been estimated by using experimental speed of sound and density values. Excess properties were fitted to the Redlich-Kister polynomial equation to obtain the binary coefficients and the standard errors. The molecular scale interactions between ionic liquid and alkoxyalkanols have been investigated through ¹H NMR spectroscopy. NMR chemical shifts for hydroxyl group of alkoxyalkanols and their deviations show hydrogen bonding interactions of varying strengths between ionic liquid and alkoxyalkanol in their binary mixtures.     

Manumycin的2D NMR研究

应用1D NMR 和梯度2D NMR技术（gCOSY，gNOESY，gHSQC，gHMBC）深入研究了从链霉菌发酵物中分离提取得到的Manumycin的结构，并对其¹H和¹³C NMR化学位移进行了全归属. 计算机分子模拟与NMR研究取得一致结论.     

NMR Study of Pentafluoroaniline - Hydrogen Bonding and Proton Exchange

The temperature and concentration dependence of ¹H NMR chemical shifts of pentafluoroaniline and aniline in acetone (Ac), dimethylsulphoxide (DMSO) and hexamethylphosphortriamide (HMPA) indicate that the effect of hydrogen bond formation, δ = δ_obs - δ_A' is similar for both anilines. The analysis of ¹H NMR spectra showed, that proton exchange of t-butyl alcohol (tBA) and 2,6-di-t-butylphenol (DTBPh) with pentafluoroaniline is slower than that with aniline.     

Quantum cluster equilibrium theory of liquids: temperature dependent chemical shifts,quadrupole coupling constants and vibrational frequencies in liquid ethanol

Temperature dependent NMR chemical shifts for hydrogen and oxygen, NMR quadrupole coupling constants for deuterium and vibrational frequencies for the OH bond of liquid ethanol are calculated for the temperature range 250 to 350 K using the ab initio quantum cluster equilibrium method and compared with experimental measurements. The calculated NMR chemical shifts, quadrupole coupling constants and infrared vibrational frequencies are in good agreement with experimental measurements. The results indicate that cyclic tetramer and pentamer structures rather than linear structures are the principal components of liquid ethanol.     

吡啶衍生物研究(Ⅰ)3-(4-吡啶基)-4-烷(芳)基-1,2,4-三唑啉-5-硫酮的NMR研究

研究并归属了十七个3-(4-吡啶基)-4-烷(芳)基-1,2,4-三唑啉-5-硫酮的¹HNMR和¹³C NMR化学位移,讨论了影响化学位移的主要因素.     

红外光谱法和量子化学法对离子液体提取水中壬基酚的机理研究

采用红外光游法和毓子化学计算法(密度泛函B3LYP方法),分别对常见离子液体1-甲基-3-丁基咪唑六氟磷酸盐和含羟基的咪唑型离子液体提取水环境中的壬基酚的提取机理进行了研究.研究结果显示常见离子液体与壬基酚相互作用前后的红外谱图上没有氢键存在的迹象,而含羟基的离子液体在与壬基酚作用后其羟基峰发生了明显的红移.量子化学计...     

含手性轴的季戊四醇双缩醛的NMR研究

采用1D和2D梯度场NMR技术(包括1D ¹H NMR, ¹³C NMR, DEPT, 2D ¹H-¹H COSY, HSQC, HMBC),对3,3′-二（2,4-二氯苯基）-2,4,2′,4′-四氧杂螺[5.5]十一烷的4个亚甲基呈现的4组裂分峰进行了明确的归属,也对化合物中其它¹H和¹³C NMR谱信号进行了全归属,为四氧杂螺双缩醛类化合物的结构鉴定提供了充分依据.     

环维黄杨星D^13C和^1H化学位移的全归属

环维黄杨星D为自黄杨木中提取精制的有效生物碱,临床上已长期用于心血管疾病的治疗.本文用制备高效液相色谱提取、分离并纯化环维黄杨星D,用1D,2D NMR技术 (COSY,DEPT,HMQC 和 HMBC)对其结构进行研究,并且首次对环维黄杨星D的1H NMR 和 13C NMR 信号进行了全归属,同时通过NMR数据确证了环维黄杨星D的结构.     

Fluorine NMR Chemical Shifts in Certain Ionic Fluorides

NMR chemical shifts are known for various nuclei in numerous solid compounds. Especially detailed data were obtained for NMR of ¹⁹F. The present work cites the measurement results for fluorine NMR chemical shifts in several d¹⁰-element fluorides previously not investigated. At the same time, the fluorine chemical shift values in alkali, alkali-earth and some other metal fluorides were measured anew. (This was necessitated by the discrepancies in the shift magnitudes, cited by various authors, as well as by the inaccuracy of the mutual chemical shifts of some standards commonly used.     

Using liquid and solid state NMR and photoluminescence to study the synthesis and solubility properties of amine capped silicon nanoparticles

Water soluble silicon nanoparticles were prepared by the reaction of bromine terminated silicon nanoparticles with 3-(dimethylamino)propyl lithium and characterized with liquid and solid state nuclear magnetic resonance (NMR) and photoluminescence (PL) spectroscopies. The surface site dependent 29Si chemical shifts and the nuclear spin relaxation rates from an assortment of 1H-29Si heteronuclear solid state NMR experiments for the amine coated reaction product are consistent with both the 1H and 13C liquid state NMR results and routine transmission electron microscopy, ultra-violet/visible, and Fourier transform infrared measurements. PL was used to demonstrate the pH dependent solubility properties of the amine passivated silicon nanoparticles.