Crystal,Molecular, and Electronic Structure of 1-Acetyl-indoline and Derivatives

The crystal and molecular structures of the following molecules have been determined: 1-acetyl-indoline, 1-acetyl-5-nitro-indoline, l-acetyl-5-nitro-7-bromo-indoline, 1-acetyl-5-bromo-7-nitroindoline, and l-acetyl-5-bromo-7-nitro-indol. Molecular orbital calculations are performed for these compounds and two related species.     

合成重要中间体1,4位官能化化合物的简便方法

5,6-取代环烯醚2在乙腈的单重态氧反应有效的生成一系列1,4位官能化化合物3。1,4位官能化化合物为合成上重要的中间体。环烯醚2可以通过β-二酰基化合物1和1,3-二溴丙烷在稀碱(碳酸钾/丙酮)条件下缩合生成。     

Preparation, characterization and thiol-thione tautomeric studies of 2-thiono-4-methyl-5-(2,2,2-trifluoro-1-trifluoromethylethyl)-1,3-thiazoline

The synthesis of a new trifluoromethyl 2-mercapto-1,3-thiadiazole derivative from 5,5,5-trifluoro-4-(trifluoromethyl)-3-penten-2-one, its structural study in the solid state and in the liquid phase and the thiol-thione tautomeric equilibrium study of the title compound are reported. The crystalline structure shows short intermolecular FF contacts. Theoretical calculations using HF and DFT methods were performed. Vibrational spectra were calculated for both tautomers and compared with experimental data. The experimental and theoretical results can be interpreted in terms of the existence of a thione tautomer in the solid and in solution.     

Thermochromism in nickel(II) complexes: thermal, solid state H NMR and single crystal X-ray analysis of bis-(N,N-dimethyl-1,2-ethanediamine) nickel(II) perchlorate

The complex bis-(N,N-dimethyl-1,2-ethanediamine) nickel(II) perchlorate undergoes a first-order thermochromic phase transition at ca. 476 K, changing its color from orange to red. The room temperature X-ray crystal structure determination showed that the nickel ion possesses a square-planar geometry with two five membered chelate rings, in the δλ conformation, forming the NiN₄ chromophore. The broad-line ¹H NMR indicates the onset of a dynamic disorder of diamine chelate rings at the phase transition temperature region, while T₁ measurement of ¹H affords the activation energy of the puckering metal chelate rings to be 26 kJ mol⁻¹. The electronic spectrum revealed that a weakening of ligand field around the nickel is associated with the phase transition.     

Synthesis of (±)-pseudoheliotridane by allylboration of 1-pyrroline

Reaction of tricrotylborane with 1-pyrroline proceeds stereoselectively to give (1R ^* ,1′S ^* )-2-(1-methylallyl)pyrrolidine. The latter was converted to the pyrrolizidine alkaloid (±)-pseudoheliotridane through hydroboration-oxidation-intramolecular cyclization. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1450–1452, July, 1998.     

Selective synthesis of di(propen-1-yl)sulfone and di(propen-1-yl)sulfoxide

Convenient selective methods of synthesis of the title compounds, based on oxidation of di(propen-1-yl)sulfide with 30% H₂O₂, have been developed.Institute of Organic Chemistry, Siberian Branch, Russian Academy of Sciences, 664033 Irkutsk. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 3, pp. 675–679, March, 1992.     

二羟基丙酮磷酸酯的合成

本文报道由3-氯-1,2-丙二醇(1)经七步反应,合成二羟基丙酮磷酸酯缩乙酮(7)的方法,总收率43%。在温和条件下,7可以水解为游离的二羟基丙酮磷酸酯(8)。     

On Deciding between Space Groups Pnam and Pna21 for the Crystal Structure of Zr3N4

The crystal structure of Zr₃N₄ is shown to crystallize in the centrosymmetric space group Pnam rather than in the noncentrosymmetric space group Pna2₁.     

Synthesis and Crystal Structure of N,N''''-Diphenyl-3, 6-diethyl-1,4-dihydro-s-tetrazine-1,4-dicarbonamide

1INTRODUCTIONIthasbeenarousedmoreandmoreinterestsinces-tetrazinewasfirstsynthesizedbyHautgschin1900[1].Thesynthesisofdihydroderivativeof3,6-dimethyl-s-tetrazinewasreportedindetailbySkorianetz[2].UsingX-ray,Jennison[3]foundthat1,6-dihydro-s-tetrazinehashom…     

对氟苯酚-过氧化氢-辣根过氧化物酶体系酶联荧光免疫分析研究──Ⅰ.对氟苯酚直接法及铝-钙指示剂偶合法测定人血清中乙肝表面抗原和表面抗体

对氟苯酚在辣根过氧化物酶（HRP）的催化下可被H2O2氧化，生成本酚及F-。测定对氟苯酚荧光猝灭程度及用铝－钙指示剂荧光体系检测酶促反应释放的F－，可分别建立HRP及其标记物的两种分析方法。铝－钙指示剂偶合法测定HRP的线性范围为0．031～31U／L，检测限（3δ）为0．0093U／L。两种方法分别用于测定人血清中乙肝表面抗原及抗体，结果令人满意。