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1.
The syntheses of (±)-curcuphenol 1, (±)-curcudiol 2, (±)-curcuhydroquinone 3, and (±)-curcuquinone 4 have been achieved. The key steps involved in the syntheses were the Reformatsky reaction and hydrogenation reaction. 相似文献
2.
A full account of the total synthesis of (±)-maistemonine, (±)-stemonamide, and (±)-isomaistemonine is presented. Two approaches have been developed to construct the basic pyrrolo[1,2-a]azepine core of the Stemona alkaloids, featuring a tandem semipinacol/Schmidt rearrangement of a secondary azide and a highly stereoselectively desymmetrizing intramolecular Schmidt reaction, respectively. To build the common spiro-γ-butyrolactone, a new protocol was carried out by utilizing an intramolecular ketone-ester condensation as the key transformation. The vicinal butyrolactone moiety of (±)-maistemonine was stereoselectively introduced via a one-pot procedure involving the epimerization at C-3 and carbonyl allylation/lactonization. Moreover, (±)-stemonamide was divergently synthesized from a common intermediate, and (±)-isomaistemonine was obtained via the epimerization of (±)-maistemonine at C-12. 相似文献
3.
2,3,9,10-Tetraoxygenated protoberberine alkaloids (14) were efficiently synthesized from the readily available benzaldehyde (2 or 10) via the benzylphenethylamines (11) and 2-phenethylisoquinolin-3-ones (12 and 13). 相似文献
4.
The compound Ba4Fe2I5S4 has been prepared at 1223-1123 K by the "U-assisted" reaction of FeS, BaS, S, and U with BaI2 as a flux. A more rational synthesis was also found; however, the presence of U appears to be essential for the formation of single crystals suitable for X-ray diffraction studies. Ba4Fe2I5S4 crystallizes in a new structure type with two formula units in space group I4/m of the tetragonal system. The structure consists of a Ba-I network penetrated by (1)infinity[Fe2S4] chains. Each Fe atom, which is located on a site with 4 symmetry, is tetrahedrally coordinated to four S atoms. The FeS4 tetrahedra edge-share to form linear (1)infinity[Fe2S4] chains in the [001] direction. The Fe-Fe interatomic distance in these chains is 2.5630(4) A, only about 3% longer than the shortest Fe-Fe distance in -Fe metal. Charge balance dictates that the average formal oxidation state of Fe in these chains is +2.5. The M?ssbauer spectra obtained at 85 and 270 K comprise a single quadrupole doublet that has hyperfine parameters consistent with an average Fe oxidation state of +2.5. The M?ssbauer spectrum obtained at 4.2 K consists of a single magnetic sextet with a small hyperfine field of -15.5 T. This spectrum is also consistent with rapid electron delocalization and an average Fe oxidation state of +2.5. The molar magnetic susceptibility of Ba4Fe2I5S4, obtained between 3.4 and 300 K, qualitatively indicates the presence of weak pseudo-one-dimensional ferromagnetic exchange within a linear chain above 100 K and weak three-dimensional ordering between the chains at lower temperatures. 相似文献
5.
Excitation functions and isomeric ratios for 184Re, from -induced reactions on 181Ta and natural W have been measured using the stacked-foil method. The data are compared with the theoretical predictions provided by the equilibrium and pre-equilibrium reaction model; for this propose we used the code INDEX development by ERNST. 相似文献
6.
PCL possesses a wide range of medical applications, such as tissue engineering and controlled drug release, because of its good biodegradability and miscibility. In order to extend the use of PCL, researchers have been exploring its structural and chemica… 相似文献
7.
Trichloro- and triisopropoxy-niobium(V) and tantalum(V) alkylene dithiophosphates, (M = Nb(V) or Ta(V); G =–CHMeCHMe–,–CMe 2CMe 2–,–CH 2CMe 2CH 2–,–CH 2CEt 2CH 2–or–CMe 2CH 2CHMe–and X = Cl or OPr i) have been synthesized by reaction of metal(V) chloride, MCl 5, or triisopropoxymetal(V) dichloride, (Pr iO) 3MCl 2, with the sodium salts of O,O′-alkylene dithiophosphoric acids, in 1 : 2 molar ratio in THF under anhydrous conditions. These pink-purple or light-yellow compounds are viscous, semi-solid or solid, hydrolyzable and soluble in common organic solvents. These compounds have been characterized by elemental analyses, molecular weight determinations and spectral studies like IR and heteronuclear NMR ( 1H, 13C and 31P), which indicated a bidentate mode of chelation of dithio ligands, leading to a pentagonal bipyramidal geometry around the niobium(V) or tantalum(V) centers. 相似文献
8.
CuLCl, CuL 1Cl, PdLCl 2, and PdL 1Cl 2 complexes [L and L 1 being (+)-camphor and (–)-carvone thiosemicarbazones, respectively] have been synthesized. The structure of binuclear [Pd 2L 22Cl 4] complex has been determined by means of X-ray diffraction. The L 2 ligand (dehydrogenated (–)-carvone thiosemicarbazone) is coordinated via the bridging S atom to two Pd atoms. The complexes of Cu(I) and Pd(II) presumably have polynuclear and binuclear structure, respectively. These facts are in good agreement with IR and NMR spectroscopy as well as mass spectrometry data which indicate the coordination of L and L 1 ligands via the S atom. The influence of L 1 and PdL 1Cl 2 on viability of the Hep2 cell line has been studied. The PdL 1Cl 2 complex is more cytotoxic than L 1 ligand. 相似文献
9.
The electronic absorption (EAS) and fluorescence spectra and electrocatalytic and photoelectrochemical characteristics of
mixed-ligand complexes of zirconium(IV) and hafnium(IV) based on phthalocyanines in solutions and in thin films were investigated.
It was established that a significant bathochromic shift of the Q band and redistribution of the intensities in the absorption
bands are observed in the electronic absorption spectra. It was shown that films of the synthesized compounds are promising
for use as photosensitizers and electrochemical sensors for oxygen in solution.
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Translated from Teoreticheskaya i éksperimental’naya Khimiya, Vol. 44, No. 3, pp. 133–137, May–June, 2008. 相似文献
10.
Abstract Reactions of O,O′-dialkyl and alkylene dithiophosphoric acids with bis (cyclopentadienyl) titanium(IV) and zirconium (IV) dichloride in a 1:1 molar ratio in refluxing benzene proceeds with elimination of HCl and formation of the substituted derivatives, Cp 2MCl[S 2P(OR) 2] (where R = Et, Pr-n, Pr-i, Bu-i and Ph), Cp 2MCl[S 2POGO] (where G = ?CH 2CMe 2CH 2?, ?CH 2CEt 2CH 2? and ?CMe 2CMe 2?), (M = Ti and Zr). The complexes are dark red and yellow solids, soluble in common organic solvents and monomeric in nature. These have been characterized on the basis of elemental analyses, molecular weight determinations, IR, and NMR ( 1H, 13C, and 31P). GRAPHICAL ABSTRACT 相似文献
11.
Four new ternary complexes of Cu II with l-methionine and the nucleotides 5AMP (adenosine 5-phosphate), 5GMP (guanosine 5-phosphate) and 5IMP (inosine 5-phosphate), and with l-tryptophan and 5AMP, were synthesized and characterized by elemental analysis and i.r. spectroscopy. One ternary complex of N II with l-cysteine and 5IMP was also prepared and characterized. The study of the three ternary compounds of Cu II, of general formulae Cu-5NMP-l-methionine, indicates coordination of the phosphate group and of N(7) of the purinic ring. l-Methionine is bound by the carboxylic and amino groups. The ternary complex obtained from a mixture of Cu-5AMP and l-tryptophan is a dimer in which the nucleotide bridges the two copper atoms. In the complex of Ni-5IMP and l-cysteine, the nucleotide seems to bind the metal through the N(7) of the heterocyclic ring, and the l-cysteine is coordinated as a bidentate chelate by the carboxyl and thiol groups. E.s.r. spectra of the copper complexes are in good agreement with the low symmetry structure proposed. The one-electron reduction potentials E c(Fc +/Fc) (V) of Cu II to Cu I were established for the four copper complexes from cyclic voltammetry studies. The one-electron oxidation potential E a(Fc +/Fc +) (V) of Ni II to Ni III was also measured for the nickel complex. 相似文献
12.
1 INTRODUCTION Tri-butyl phosphate (TBP) has been widely used as the extraction reagent in U-Th fuel to separate uranium from thorium. But di-butyl phos- phate (DBP) and butyl phosphate (MBP), the radio- lytic products of TBP, exhibit some coordinated ability to the fission elements, such as Zr and Nb. The substitutes for TBP have being studied for several decades[1~4]. The physical and chemical properties of amides are similar to those of TBP and they selectively extract U(Ⅵ… 相似文献
13.
A reaction of [(η 5-C 6H 7)Fe(CO) 3]BF 4 with KI in acetone gave brown crystals of the complex [(η 5-C 6H 7)Fe(CO) 2] I ( I), which was treated with SnCl 2 in THF to form orange crystals of the complex [(η 5-C 6H 7)Fe(CO) 2]SnCl 3 ( II). A reaction of complex II with potassium cymantrenecarboxylate ((CO) 3MnC 5H 4COOK, or CymCOOK) in THF yielded yellow crystals of the complex [(η 5-C 6H 7)Fe(CO) 2]Sn(CymCOO) 3 ( III). Structures I–III were identified using X-ray diffraction. The fragment (η 5-C 6H 7)Fe(CO) 2 in complexes I–III remains virtually unchanged. The Fe-I bonds in complex I (2.6407(3) Å) and the Fe-Sn bonds in complexes II and III (2.4854(3) and 2.4787(4) Å, respectively) are appreciably shorter than the sum of the covalent radii of the corresponding elements, probably because of an additional dative interaction of the d electrons of iron with the vacant d orbitals of iodine or tin. 相似文献
15.
Heating of a solution of pentaphenylantimony in toluene in atmospheric oxygen affords -oxo-bis(tetraphenylantimony) ( I) in a 63% yield. The latter compound can be converted to bis(tetraphenylantimony) carbonate or phthalate by the action of carbon dioxide or phthalic anhydride, respectively. According to X-ray diffraction data, the antimony atoms in compound Ihave a distorted trigonal-bipyramidal coordination (Sb–O 2.0050(4) Å, the SbOSb angle 151.71(9)°). The molecule of bis(tetraphenylantimony) phthalate is composed of two equal fragments, and its Sb atoms also have trigonal-bipyramidal coordination (Sb–O 2.2421(8) Å; Sb–C 2.176(1), 2.115(1), 2.130(1), and 2.137(1) Å). 相似文献
16.
-Cyclodextrin (-CD) is a cyclic oligosaccharide, composed of ten -1,4-linked D-glucoses reported by French et al. in 1965 1), but has not been studied because of the difficulty in the preparation and purification of large-ring CDs composed of more than nine -1,4-linked D-glucose units. This report describes the purification and characterization of -CD. Furthermore, the crystal and molecular structure of -CD hydrate -CD 19H 2O) was elucidated by X-ray analysis. 相似文献
17.
In this study, a mononuclear CuL complex was prepared by the use of bis-N,N′-(salicylidene)-1, 3-propanediamine (LH2) and Cu2+ ion. NiCl2 and NiBr2 salt were treated with this complex in dioxanewater medium and two new complexes [(CuL)2NiCl2(H2O)2] and [(CuL)2NiBr2(H2O)2)] with Cu(II)–Ni(II)–Cu(II) nucleus structure were obtained. In addition to this bis-N,N′-(2-hydroxybenzyl)-1,3-diaminopropane (LHH2) was prepared by the reduction of LH2 with NaBH4 in MeOH medium. The treatment of this reduced complex with Cu2+ ion resulted a complex [(CuLH)2CuCl2] with a structure of Cu(II)–Cu(II)–Cu(II). The complexes prepared were characterized by the use of elemental analysis, IR spectroscopy, thermogravimetric and X-ray diffraction methods. The crystal structures of [(CuL)2NiBr2(H2O)2] (СIF file CCDC 1448402) and [(CuLH)2CuCl2] (СIF file CCDC 1448401) complexes were elucidated. It was found that halogen ions are coordinated to terminal Cu2+ ions which are in a distorted square pyramid coordination sphere. It was determined that the central Cu(II), which joins terminal square pyramidal Cu(II), was coordinated only by the phenolic oxygens of the ligand while the central Ni(II) was coordinated by two phenolic oxygens of the organic ligand and two water molecules. These complexes were investigated by XPS and it was found that the terminal and central Cu2+ ions were different in Cu(II)–Cu(II)–Cu(II) complex. Also, the thermal degradation of the CuLH complex unit was observed to exothermic in contrast to the expectations. 相似文献
19.
The title compound has been synthesized and characterized by elemental analysis and conductivity studies. The crystal and molecular structure has been determined. There are two different types of molecules in the crystal: mono- and diaquadi(acetato- O)- bis(2,4'-bipyridyl) copper (II). Both copper atoms occupy special positions. The copper atoms show almost ideal square pyramidal (4 + 1) and square bipyramidal (4 + 2) coordination. Due to the Jahn-Teller effect, the axial Cu-O(water) bond distances are longer than respective equatorial Cu-O(acetate) bond distances. The bond valences of the copper were computed. An intramolecular strong hydrogen bond linking O(water) and O(acetate) atoms exists in the molecule. The differences of geometrical environment for copper in mono- and diaquadi(acetato- O)- bis(2,4'-bipyridyl) copper(II) are imposed by strong intermolecular hydrogen bonds creating a linear infinite chain structure along crystallographic x axis. Also weak intramolecular hydrogen bonds are present in the molecule. 相似文献
20.
This paper focuses on the identification of the composition of the coverings and pigments of two archaeological sites. The sites researched here lie in Andalusia and show two contexts, which have a highly symbolic and ritual meaning. The first, Convento 2 (Montemayor, Córdoba), dates back to the period of formation of the Iberian Culture (VIIth century b.c.). The second is the cemetery of Tutugi (Galera, Granada), of the mid-Iberian period (IVth century b.c.). The analytical procedure consisted in combined and complementary use of XRD and MRS. This allowed to identify the materials used, namely hematite, goethite, coal, gypsum and calcite. Identification of these materials proves essential for the restoration and musealization of both archaeological sites. 相似文献
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