Sulphamic Acid （H2NSO3H）-Catalyzed Multicomponent Reaction of β-Naphthol： An Expeditious Synthesis of Amidoalkyl Naphthols

Sulphamic acid （H2NSO3H） was found to be an efficient catalyst for the multicomponent condensation reaction of β-naphthol, aromatic aldehydes and urea or amides to afford the corresponding α-amidoalkyl-β-naphthols in good yields. The remarkable features of this new procedure are high conversions, short reaction time, clean reaction profiles and simple experimental and work-up procedures.     

Solvothermal Synthesis and Structure Studies of a Mixed-valence Oxochloromolybdenum Complex

Emerald green crystals of a new mixed-valence oxochloromolybdenum complex,Mo(OH)2(2,2′-bipy)Cl2.[MoO(2,2′-bipy)Cl3]2, were obtained in an attempt to synthesize the Mo-S cluster compounds under solvothermal conditions. The title compound was characterized by EPR and X-ray single-crystal diffraction techniques. Crystallographic data: orthorhombic, space group Fdd2, a = 12.684(1), b = 21.518(2), c = 29.096(3)A, Mr = 1103.97, V= 7941(1)A^3, Z= 8, Dc =1.843 g/cm^3,μ= 1.514 mm^-1, F(000) = 4304, R = 0.0654 and wR = 0.1544 for 1944 observed reflections with 1 ≥/ 2σ(I). The compound consists of two different neutral molecules, Mo^IV-(OH)2(2,2′-bipy)Cl2 and MoVO(2,2′-bipy)Cl3. Both Mo^IV and Mo^V ions are in a distorted octahedral environment. The Mo(1)^IV atom is surrounded by two Cl^- ions and two O atoms from OH^- and two N atoms from a 2,2′-bipy ligand. The Mo(2) atom is surrounded by three Cl^- ions, one O^2- anion and two N atoms from another 2,2“-bipy ligand. The bipyridine occupies two cis-equatorial sites, while the Cl^- ions are located at the axial and equatorial positions.     

芳香醛与硫代巴比妥酸固相缩合反应的研究

研究了芳香醛与硫代巴比妥酸固态加热及室温下的缩合反应，两种反应条件得 到同一产物——5—亚烃基硫代巴比妥酸．由^1H NMR，^13C NMR，IR，UV等手段确 定了产物的结构．     

新的手性源5-(1- 氧基)-3,4-二氯-2(5H)-呋喃酮的合成及结构

近年来,γ-取代基α,β-不饱和丁烯内酯的合成及结构性能引起了有机化学界很大的兴趣和重视^[1],由于2(5H)-呋喃酮作为一个结构组分广泛地存在于天然产物中[2],同时也被用作有机合成的中间体^[3].新近,Feringa等^[4]利用4-羟基丁烯内酯与1-薄荷醇的脱水反应,制得了光学纯5-(1- 氧基)-2(5H)0呋喃酮并用于有机合成.我们在此基础上,改进了 4-羟基丁烯内酯的光化学制备方法;探讨了5-(1- 氧基)-2(5H)-呋喃酮的热稳定性及质子催化下差向异构化作用;并进行了不对称Michael加成^[5]和1,3-偶极环加成反应的研究^[6].本文在此基础上,深入探讨了新的手性源5-(1- 氧基)-3,4-二氯-2(5H)-呋喃酮的合成以及有关的反应.由于制备方法简便,化学产率较高,光学纯度单一,天然手性助剂薄荷醇来源方便以及γ- 氧基立体专一性控制,它为进一步合成系列新的光学活性化合物提供了有效的途径.     

毛细管气相色谱法同时测定挥发性卤代烃及氯代苯

本文报道用毛细管气相色谱法同时测定挥发性卤代烃及氯代苯。采用吹扫-捕集法富集样品，应用大口径厚液膜弹性石英毛细管柱分离，方法操作简便，准确度和重现性好，且受水样基体干扰小。     

Cp2TiCl2/i-BuMgBr还原断裂Se—Csp键反应研究

Cp₂TiCl₂/i-BuMgBr体系形成的钛氢化试剂与炔硒醚反应生成端炔与深蓝色钛硒化物, 后者在空气中被氧化为二醚, 与酰氯反应, 高产率地形成对应的硒代酯.     

Two Novel Isomers of HPS3 System

Two new isomers of HPS3 system, FIP(S)S2 and HSSPS, are predicted by means of B3LYP method with 6-311 G(3df,3pd) basis set. The two isomers can isomerize into thermodynamically the most stable species HSPS2, which have been experimentally identified,with relatively higher reaction barriers. In view of their higher thermodynamical and kinetic stability and the experimental observation for I-IP(O)O2 and HOOPO in previous study, we can reasonably believe that the two species can be spectrosymmetrically characterized in future experiments.     

用Benson基团加和法预测气相色谱保留值

应用Ｂａｎｓｏｎ基团加和法，对氯代苯，脂肪醇两类化合物分子结构与气相色谱保留值间的关系进行了研究。对部分化合物的保留值做了预测，结果表明这两类化合敢相色谱保留值具有基团加和性，预测值与实验值吻合很好。     

二硫代钨酸铵晶体的合成、表征与热分解机理的研究

本工作用偏钨酸铵和硫化铵为原料，在水溶液中合成二硫代钨酸铵晶体[(NH₄)₂WO₂S₂]。用紫外-可见光谱(UV-Vis)的方法研究了二硫代钨酸铵晶体的形成机理。采用元素分析、X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、激光拉曼光谱(LRS)等对化合物进行了表征。结果表明采用该方法制备出的二硫代钨酸铵晶体，晶型良好。热重-差热分析(TG-DTA)、原位X射线衍射(in situ XRD)和FTIR等结果表明二硫代钨酸铵晶体在氢气气氛下的热分解主要发生在160～450 ℃之间，分两步进行，首先分解为{WOS₂}，随后转化为二硫化钨。     

我国建成世界第一条氯代苯酐生产线

不久前，由中国科学院长春应用化学研究所和大连瑞泽农药股份有限公司合建的大连瑞泽聚酰亚胺有限公司，在大连建成了一条由邻二甲苯经过氯气氯代、空气气相氧化和异构体分离步骤合成氯代苯酐的500t规模生产线，这是世界上第一条氯代苯酐生产线，解决了我国聚酰亚胺生产原料的来源问题，并大大降低了生产成本。