红霉素A9-（1-异丙氧基环已基）肟的合成及其晶体结构

合成表征了红霉素A9-（1-异丙氧基环已基）肟的E和Z异构体，并在丙酮-水混 合溶液中培养出了前者的单晶，X射线衍射表明，其结构为正交晶系，P2_12_12_1 空间群，晶胞参数：a=2.3101(5) nm, b=2.3761(5) nm, c=0.97066(19)nm, V=5. 3279(8) nm~3，Z=4，μ=0.088 mm~(-1)，F(000)=2064, D_c=1.176 g/cm~3。E-红 霉素A 9-（1-异丙氧基环已基）肟的晶体结构图明显表明1-异丙氧基环已基保护基 确实使十四元大环的构象发生了扭曲，使6-OH的周围空间不再拥挤，从而导致6- OH甲基化的选择性提高。     

A Novel Reductive Cyclization of o-Nitrobenzamides and Ketones Promoted by Low-valent Titanium Reagent

A short and facile synthesis of a series of 1,2-dihydroquiazolin-4(3H)-ones was accomplished in good yields via novel reductive cyclization of o-nitrobenzamides with ketones promoted by TiCI4/Zn system. The structure was established on the basis of elemental analysis, IR,^1H NMR and confirmed by a single-crystal X-ray diffraction analysis. This method has the advantages of easily accessible starting materials, convenient manipulation and moderate to high yields.     

室温固相反应一步合成N-亚水杨基-4-氨基安替比林

4-氨基安替比林与水杨酬醛通过室温固相反应合成N-亚水杨基-4-氨基安替比 林，反应无溶剂，15 min即可完成，产率达95%，用元素分析，IR，~1H NMR，X射 线粉末衍射和X射线单晶衍射对产物进行了表征。     

含呋喃环Schiff碱型大环化合物的合成及其与Ba^2+,Sr^2+配合行为

利用Mn^2+，Ba^2+及Sr^2+作为模板离子，合成了一类新型的含呋喃环系 Schiff碱型大环化合物，如L^1和配合物L^2Ba(ClO4)2，L^3Ba(ClO4)2和L^4Ba (ClO4)2.L^2-L^4的Ba^2+配合物经与NaSO4水溶液反应解络，得到自由配体L^2， L^3和L^4，配体L^2和L^3分别与Sr^2+作用，得到配合物L^2Sr(ClO4)2和L^3Sr (ClO4)2。上述大环配体和各种配合物均经元素分析，IR，^1H NMR，MS等证实了它 们的结构和组成。     

异丙氧基-异羟肟酸-氧钒（V）配合物的合成、晶体结构和量子化学研究

以苯甲酰异羟肟酸为配体，首先合成四价氧钒化合物，以此为基础合成了标题 化合物，并用元素分析，红外光谱，~1H NMR，~(13)C NMR，~(15)V NMR，电子吸 收光谱等，分别对它进行了表征，其结构用单晶X射线衍射法测定，晶体属三斜晶 系，P1-bar空间群，所得晶体学参数为a = 1.1119(3) nm，b = 1.1735(3) nm，c = 0.8660(2) nm，α = 96.84(1)°，β = 106.93)(1)°，γ = 88.97(1)°，V = 1.0731(2) nm~3，D_c = 1.415 g/cm~3，Z = 2，F(000) = 478，μ = 5.06 cm~(-1)。采取ab initio(GTO-6-31d)方法对标题化合物的结构单元的成键情况进 行了分析，讨论了化合物的稳定性、分子轨道能量、原子静电荷分布等情况。     

α-羰基硫代甲酰胺与溴的反应研究

报道了α 羰基硫代甲酰胺与溴在三乙胺存在下的反应 ,合成了二 [( 1 芳基亚胺基 1 苯甲酰基 )甲基 ]二硫醚类化合物 ,产率为 60 %～ 65 %.它们的结构经元素分析、红外光谱、核磁共振光谱和质谱分析得到确证     

蛋氨酸合成酶催化反应研究Ⅴ：5-氨基-6-（3-羟基-4-溴丁基）尿嘧啶的合成研究

报导了5-氨基-6-（3-丁烯基）尿嘧啶、5-氨基-6-（3-羟基-4-溴丁基）尿嘧 啶的合成方法。以γ-取代的β-酮脂和O-甲基异尿硫酸盐为超始物，经6-取代尿嘧 啶（3）、6-取代-5-偶氮尿嘧啶（4）和未见文献报道的中间体6，首次合成了5-氨 基-6-（3-丁烯基）尿嘧啶（5）及5-氨基-6-（3-羟基-4-溴丁基）尿嘧啶（7）。     

On the Criteria of Instability for Electrochemical Systems

Both cyclic-voltammetry-based and impedance-based experimental criteria that have been developed recently for the oscillatory electrochemical systems are critically appraised with two typical categories of oscillators.Consistent conclusions can be drawn by the two criteria for the category of oscillators that involve the coupling of charge transfer mainly with surface steps(e.g.ad-and desorption)such as in the electrooxidation of C1 organic molecules.Whereas,impedance-based criterion is not applicable to the category of oscillators that involve the coupling of charge transfer mainly with mass transfer(e.g.diffusion and convection) such as in the Fe(CN)6^3- reduction accompanying periodic hydrogen evolution.The reason is that the negative impedance cannot include the feedback information of convection mass transfer induced by the hydrogen evolution.However,both positive and negative nonlinear feedbacks,i.e., the diffusion-limited depletion and convection-enhanced replenishment of the Fe(CN)6^3- surface concentration,that coexist between the bistability,i.e.,Fe(CN)6^3- reduction with and without hydrogen evolution at lower and higher potential sides respectively,are all reflected in the crossed cyclic voltammogram(CCV).It can be concluded that the voltammetry-based criterion(in time domain)is more intuitive,less time-consuming and has a wider range of applications than the impedancebased one (in frequency domain).     

Investigation on False Peak Phenomena in On-line Sweeping Technique in MEKC

ＩｎｔｒｏｄｕｃｔｉｏｎＭｉｃｅｌｌａｒｅｌｅｃｔｒｏｋｉｎｅｔｉｃｃｈｒｏｍａｔｏｇｒａｐｈｙ (ＭＥＫＣ)ｗａｓｉｎｖｅｎｔｅｄｔｏｅｘｔｅｎｄｔｈｅｕｔｉｌｉｔｙｏｆｃａｐｉｌｌａｒｙｅｌｅｃｔｒｏｐｈｏｒｅｓｉｓ(ＣＥ)ａｎｄｐｅｒｍｉｔｔｅｄｔｈｅｓｅｐａｒａｔｉｏｎａｎｄａｎａｌｙｓｉｓｏｆｎｅｕｔｒａｌｃｏｍｐｏｕｎｄｓ .ＢｕｔｊｕｓｔｌｉｋｅｏｔｈｅｒｍｏｄｅｓｏｆＣＥ ,ＭＥＫＣａｒｅｈａｍｐｅｒｅｄｂｙｔｈｅｌｏｗｃｏｎｃｅｎｔｒａｔｉｏｎｓｅｎｓｉｔｉｖｉｔｙｏｆｔｈｅｕｌｔｒａ …     

Study on Tonghaosu and Its Analogs： Isolation, Structure Identification and Synthesis of Antifeedant B-ring-homo-tonghaosu

The methanolic extract from a Chinese endemic Chrysanthemum plant, Dendranthema indicum var. aromaticum, was found to show high antifeeding activity against Pieris brassicae L., and by bioassay-guided separation, the active component, B-ring-homo-tonghaosu, 2-(2‘,4‘-hexadiynylidene)-1,6-dioxaspiro-[4,5]-dec-3-ene (2) was isolated. Its structure was elucidated by comparing its spectroscopic data with those of 2 reported in the literatures. Furthermore new convenient total synthesis methods of B-ring-homo-tonghaosu were also developed to confirm its structure and make its further application in crop protection available. In addition, extensive comparison of spectroscopic data showed that the structure of compound 21 reported in literature should be revised to 2.