化学发光物质9-[2'',6''-二甲基-4''-(琥珀酰亚胺氧羰基)苯氧羰基]-10-甲基吖啶-单甲基-磺酸盐的合成

报道了一种化学发光物质吖啶酯衍生物9-[2',6'-二甲基-4'-(琥珀酰亚胺氧羰基)苯氧羰基]-10-甲基吖啶-单甲基-磺酸盐(DMAE·NHS)的合成,合成共经历7个步骤,每步合成的产物经IR,1H NMR,MS和元素分析表征,结果表明合成产物为所期望的化合物.该合成产物显示为一种非常理想的化学发光物质.     

钯碳催化法合成4,4'-二甲基-2,2'-联吡啶

以4-甲基吡啶为原料, 钯碳催化合成了4,4'-二甲基-2,2'-联吡啶. 通过¹H NMR, GC-MS, 元素分析对产物进行了表征, 对催化反应进行了分析, 并且讨论了钯碳催化反应的机理.     

化学发光免疫分析试剂吖啶酯的合成新路线

设计了一种化学发光免疫分析试剂吖啶酯的合成新路线,以二苯胺为原料合成吖啶-9-羧酸,经酰氯化后与3-(4-羟基苯基)-丙酸-N-羟基琥珀酰亚胺酯反应得4-(2-琥珀酰亚胺基氧羰基乙基)苯基-9-吖啶羧酸酯,最后与氟磺酸甲酯反应即得4-(2-琥珀酰亚胺基氧羰基)苯基-10-甲基吖啶-9-羧酸酯氟磺酸盐(俗称吖啶酯).     

10,10’-二甲基-3,3’-二磺酸基-9,9’-双吖啶的电致化学发光行为

研究了新试剂10,10'-二甲基-3,3'-二磺酸基-9,9'-双吖啶(简称DMDSBA)的电致化学发光(ECL)行为. 考察了电化学参数、反应介质以及pH等条件对DMDSBA电致化学发光信号的影响. 结果表明, 在玻碳电极上施加适当电压时, DMDSBA在KNO₃溶液介质中产生很强的电化学发光信号, 于优化的实验条件下, 发光强度的自然对数与DMDSBA浓度的自然对数在1.0×10^-5-1.0×10^-8 mol·L^-1范围内呈良好的线性关系,检出限可达2.3×10^-9 mol·L^-1. 并用循环伏安法、电致化学发光光谱以及荧光光谱, 研究了DMDSBA的电致化学发光机理.     

N-(2-甲氧羰基-1-甲基)-乙基-(N′-D-乙酰基吡喃型糖)硫脲类化合物的合成及生物活性

N-(2-甲氧羰基-1-甲基)-乙基-(N′-D-乙酰基吡喃型糖)硫脲类化合物的合成及生物活性;糖基硫脲;β-氨基丁酸;合成;生物活性     

N-(2-甲氧羰基-1-甲基)-乙基-(N′-D-乙酰基吡喃型糖)硫脲类化合物的合成及生物活性

N-(2-甲氧羰基-1-甲基)-乙基-(N′-D-乙酰基吡喃型糖)硫脲类化合物的合成及生物活性;糖基硫脲;β-氨基丁酸;合成;生物活性     

6-甲氧羰基-4,4'-二甲基-2,2'-联吡啶单核铜(Ⅰ)双膦发光配合物

合成并表征了2个新的基于6-甲氧羰基-4,4''-二甲基-2,2''-联吡啶的单核铜（Ⅰ）双膦配合物[Cu（mmbpy）（dppp）]ClO₄（1）和[Cu（mmbpy）（dppb）]ClO₄（2）。研究结果表明,铜（Ⅰ）配合物1和2均表现为扭曲变形的N₂P₂四面体几何构型,其P-Cu-P键角受辅助双膦配体控制。在常温下,这2个铜（Ⅰ）配合物在固态时均具有发光性质,并且相对于双膦配体亚甲基链的长度,P-Cu-P键角对其光物理性质的影响更为显著。在2,2''-联吡啶环上引入2个甲基取代基对改善铜（Ⅰ）配合物的发光性能也被证明是有效的。     

2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-5-(取代苯基亚甲基)-4- 噻唑啉酮的合成

以2-氨基-5-取代苯氧甲基-1,3,4-噻二唑(1)为起始原料, 合成了中间体2-氯乙酰氨基-5-取代苯氧甲基-1,3,4-噻二唑)-2-乙酰亚胺(2)和2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-4-噻唑啉酮(3), 化合物3进一步与取代苯甲醛发生类Knoevenagle缩合反应, 得到了一系列2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-5-(取代苯基亚甲基)-4-噻唑啉酮类化合物4a～4p. 目标化合物4a～4p的结构经IR, ¹H NMR和元素分析确证.     

新型3-芳甲基-5-芳氧甲基丁内酯的合成及其抑制肺癌细胞生长活性评价

通过2-芳氧甲基环氧烷与α-芳甲基丙二酸二乙酯在乙醇钠条件下反应, 合成了8个新型3-芳甲基-5-芳氧甲基丁内酯, 收率为13%～81%. 由IR, ¹H NMR和MS波谱数据进行了结构表征. 所得化合物均具有抑制A549肺癌细胞生长的活性, 其抑制效果具有浓度依赖性.     

聚(Nε-苄氧羰基赖氨酸)-聚乙二醇-聚(Nε-苄氧羰基赖氨酸)的合成及其表征

利用三光气合成了Nε-苄氧羰基赖氨酸酸酐(Lys(z)-NCA),并用双端氨基聚乙二醇做引发剂,在DMF中引发Lys(z)-NCA聚合,合成了聚(Nε-苄氧羰基赖氨酸)-聚乙二醇-聚(Nε-苄氧羰基赖氨酸)三嵌段共聚物.利用IR、1H NMR、DSC和GPC对其结构进行了表征,结果表明,这种方法能够合成分子量可控、分子量分布窄(Ip=1.06)的嵌段共聚物,产率95.4%.     

Synthesis and Crystal Structure of (Z)-Ethyl 5-(phenylamino)-3-(phenylimino)-3H-1,2-dithiole-4-carboxylate

The compound (Z)-ethyl 5-(phenylamino)-3-(phenylimino)-3H-1,2-dithiole-4-carboxylate 3 has been synthesized by the reaction of ethylacetoacetate 1 and phenylisothiocyanate 2. Its structure has been established by ¹H NMR, ¹³C NMR, infrared, mass spectra, and x-ray crystallography.      

Selective Spectrophotometric Determination of Palladium (II) With 2-(5-Bromo-2-Pyridylazo)-5-(Diethylamino)-Phenol

Abstract

A spectrophotometric study of the Pd(II) complex of a reagent 2-(5-Bromo-2-Pyridylazo)-5-(diethylamino)-Phenol (5-Br-PADAP) is presented. A violet complex is formed at pH 3.53, and shows maximal absorbance at 585 nm with molar absorptivity of 3.86 × 10⁴ 1. mol^?1 cm^?1. Beer's law is obeyed up to 50 μ of Pd(II). The method offers the advantages of simplicity, high precision, requires no extraction and is very selective, where 5.0 mg Pt(VI) and 0.3 mg Au(III) ions do not interfere.     

Amberlite XAD-7 resin impregnated with 2-(1-(4-chlorophenyl)-4,5-diphenyl-1H-imidazol-2yl)-4-nitrophenol for enrichment of metal ions

The Amberlite XAD-7 resin modification was carried out by loading 2-(1-(4-chlorophenyl)-4,5-diphenyl-1H-imidazol-2yl)-4-nitrophenol (CPDPINP). Subsequently, this new sorbent was applied for the enrichment of metal ions such as Cu²⁺, Ni²⁺, Co²⁺ Zn²⁺ and Pb²⁺ ions. The effect of various parameters on their sorption and following recoveries was studied in column procedure. The preconcentrated ions were eluted by appropriate eluent and their contents were quantified by FAAS. This method has preconcentration factor of 150 and enrichment factor in the range of 20.8–29.1. At optimum values of all variables, the proposed method has linear calibration graphs in the range of 0.01 up to 0.29 μg mL⁻¹ with detection limit (3SDb/m, n = 15) between 1.6 and 2.6 ng mL⁻¹. This protocol is usable for successful analysis of Cu²⁺, Ni²⁺, Co²⁺ Zn²⁺ and Pb²⁺ ions in different matrices with reasonable recoveries (>93%) and acceptable relative standard deviation (<4.7%).     

Spectrophotometic Determination Of Tin In Steels With2-(5-Nltro-2-Pyridylazo)-5-[N-n-Propyl-N-(3-Sulfopropyl)Amino]phenol

ABSTRACT

A highly sensitive azo dye, 2-(5-nitro-2-pyridylazo)-5-[N-n-propyl-N-(3-sulfopropyl)amino]phenol (Nitro-PAPS), is used as a colorimetric reagent for the determination of tin(IV) content. Nitro-PAPS reacts with tin(IV) to form a water-soluble complex in 1.0 M acetic acid. Full color development is attained within 5 minutes, and maintains constant absorbance for at least 24 hours. The apparent molar absorptivity is 7.7 x 10⁴ dm³ mol^?1 cm^?1 at a maximum wavelength of 580 ran. Beer's law is obeyed for tin(IV) in the range of 0-1.2 μg ml^?1. The proposed method is successfully applied to the determination of trace amounts of tin in steels.     

Spectral-luminescent and solvatochromic properties of 2-(3-coumarinyl)-5-(2′-(R-amino)-phenyl)-1,3,4-oxadiazoles

Spectral-luminescent properties of the newly synthesized 2-(3^′-coumarinyl)-5-(2′-(R-amino)-phenyl)-1,3,4-oxadiazoles has been investigated in solvents of various polarity and hydrogen-bonding ability. It has been found that for all the studied compounds no excited state intramolecular proton transfer occurs despite the presence of coumarinyl fragment - electron acceptor effect of the coumarinyl fragment is not sufficient to increase the excited state acidity of the amino group. It has been found that the absorption spectra of the studied compounds shift to higher energy with increase in solvent polarity, whereas corresponding fluorescence spectra shift to lower energy with solvent polarity increase. It has been suggested that long-wavelength shifts of the fluorescence spectra of the studied compounds with increase in solvent polarity is caused by the solvent relaxation. The observed solvent relaxation effect allow us to propose some of the studied compounds as potential probes to monitor changes in solvent relaxation in low-polar media and as potential probes for rigidochromic effect.     

3-取代苄氧基-6-取代氨基哒嗪衍生物的合成及其除草活性

通过3-取代苄氧基-6-氟哒嗪在75～80 ℃与二甲胺的绝对无水乙醇溶液封管反应, 或在回流条件下分别与吗啡啉或哌啶反应, 合成一系列新颖的3-取代苄氧基-6-取代氨基哒嗪类化合物, 它们的结构均经IR, ¹H NMR和元素分析确证. 初步的除草活性测定结果表明, 该类化合物具有一定的除草活性, 讨论了它们的结构与除草活性的关系.     

1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲的合成及手性晶体结构

对二甲氨基苯甲醛和苯基氨基硫脲缩合反应生成对二甲氨基苯甲醛缩氨基苯硫脲{1-[4-(dimethylamino)ben- zylidene]-4-phenylthiosemicarbazide}, 并从溶液中析出手性晶体. 元素分析、红外光谱、紫外光谱、核磁谱、质谱和X射线衍射测定其组成和结构. 晶体属正交晶系, P2₁2₁2₁空间群, a＝0.77038(14) nm, b＝1.1428(2) nm, c＝1.6726(3) nm, V＝1.4726(5) nm³, Z＝4, D_c＝1.346 g/cm³, F(000)＝632, μ＝0.219 mm^－1, 可观测点精修最终偏离因子: R＝0.0407, wR＝0.1157. 化合物的晶体结构和固态圆二色谱表明化合物在结晶过程中发生单一对映体的手性堆积.     

Iron(III) complexes bearing 2-(benzimidazole)-6-(1-aryliminoethyl)pyridines: Synthesis, characterization and their catalytic behaviors towards ethylene oligomerization and polymerization

A series of iron(III) complexes ligated by 2-(benzimidazole)-6-(1-aryliminoethyl)pyridines was synthesized and examined by ¹H NMR, ESI-MS, IR spectroscopic, elemental analysis and X-ray photoelectron spectroscopy (XPS). Activated with methylaluminoxane (MAO), all ferric complexes exhibited good activities (up to 5.38 × 10⁶ g mol⁻¹(Fe) h⁻¹) of ethylene oligomerization and polymerization, and resultant oligomers and polyethylene waxes showed high α-olefin feature, meanwhile the distribution of oligomers mostly resembled Schulz-Flory rules. The various reaction parameters were investigated in detail, and the less bulky and electron-withdrawing substituents of ligands could enhance the catalytic activities of their ferric complexes. The observations explain the cause for unstable activities performed by stored iron(II) complexes.     

1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲的另一个手性对映体晶体结构

对-二甲氨基苯甲醛和苯基氨基硫脲缩合反应生成1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲(DMB), 产物能从溶液中析出单一手性对映体晶体. 用单晶X射线衍射技术测定了它的绝对构型, 晶体属正交晶系, P2₁2₁2₁空间群, a＝0.7870(2) nm, b＝1.1560(2) nm, c＝1.6668(3) nm, V＝1.5164(5) nm³, Z＝4, D_c＝1.307 g/cm³, F(000)＝632, μ＝0.213 mm^－1, 2557个可观测点[I＞2s(I)]精修的最终残差因子: R＝0.0409, wR＝0.1061, Flack参数为0.00(9), 能够确定绝对构型. 化合物的晶体结构和大宗粉末样品的固体圆二色谱表明化合物在结晶过程中发生单一对映体的手性堆积.