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1.
N-2-(3-picolyl)-N′-phenylthiourea, 3PicTuPh, monoclinic, P21/n, a=7.617(2) b=7.197(5), c=22.889(5) Å, β=94.63(4)°, V=1250.7(1) Å3 and Z=4; N-2-(4-picolyl)-N′-phenylthiourea, 4PicTuPh, triclinic, P-1, a=7.3960(5), b=7.9660(12), c=21.600(3) Å, α=86.401(4), β=84.899(8), γ=77.769(8)°, V=1237.5(3) Å3 and Z=4; N-2-(5-picolyl)-N′-phenylthiourea, 5PicTuPh, monoclinic, P21/c, a=14.201(1), b=4.905(3), c=17.689(3) Å, β=91.38(1)°, V=1231.8(7) Å3 and Z=4; N-2-(6-picolyl)-N′-phenylthiourea, 6PicTuPh, monoclinic, C2/c2, a=14.713(1), b=9.367(1), c=18.227(1) Å, β=92.88(1)°, V=2515.5(1) Å3 and Z=8 and N-2-(4,6-lutidyl)-N′-phenylthiourea, 4,6LutTuPh, monoclinic, C2/c, a=11.107(2), b=11.793(2), c=20.084(4) Å, β=96.10(3)°, V=2616(1) Å3 and Z=8. Intramolecular hydrogen bonding between N′H and the pyridyl nitrogen and intermolecular hydrogen bonding involving the thione sulfur are affected by substitution of the pyridine ring, as is the planarity of the molecule. 1H NMR studies in CDCl3 show the NH′ hydrogen resonance considerably downfield from other resonances in the spectrum for each thiourea.  相似文献   

2.
Three new compounds of aryl thiourea derivatives, namely N-2-(4-picolyl)-N′-(4-methoxyphenyl)thiourea (L1), N-2-(6-picolyl)-N′-(4-methoxyphenyl)thiourea (L2) and N-2-(4-picolyl)-N′-(4-nitrophenyl)thiourea (L3), and the new copper(II) complex [Cu(4PicTz4OMePh)(OAC)(EtOH)] (C1), as a result of oxidative cyclization of the ligand (L1), were synthesized. In addition, pure precursor (P1), as the product of the oxidative cyclization of N-(2-pyridyl)-N′-(4-methoxyphenyl)thiourea (L4), was isolated and characterized. Ligands (L1) and (L2) were characterized by 1H and 13C NMR and single crystal X-ray analysis. 1H NMR spectroscopy showed strong hydrogen bonding interactions between N′H-functionalities and the pyridine nitrogen atoms as well as weak intermolecular hydrogen bonding between the thione sulfur and the NH hydrogen. Structural studies of complex (C1) showed that the copper ion is five-coordinated with a square-pyramidal environment. The oxidative cyclization of ligand (L1) results in an anionic bidentate ligand in complex (C1). Both ligand (L1) and precursor (P1) crystallize as centrosymmetric dimers.  相似文献   

3.
The reactions of 1 mol equiv. each of [Ru(PPh3)3Cl2] and N-(acetyl)-N′-(5-R-salicylidene)hydrazines (H2ahsR, R = H, OCH3, Cl, Br and NO2) in alcoholic media afford simultaneously two types of complexes having the general formulae [Ru(HahsR)(PPh3)2Cl2] and [Ru(ahsR)(PPh3)2Cl]. The complexes have been characterized by elemental analysis, magnetic, spectroscopic and electrochemical measurements. Molecular structures of [Ru(HahsH)(PPh3)2Cl2] and [Ru(ahsH)(PPh3)2Cl] have been confirmed by X-ray crystallography. In both species, the PPh3 ligands are trans to each other. The bidentate HahsH coordinates to the metal ion via the O atom of the deprotonated amide and the imine–N atom in [Ru(HahsH)(PPh3)2Cl2]. In HahsH, the phenolic OH is involved in a strong intramolecular hydrogen bond with the uncoordinated amide N atom forming a seven-membered ring. In [Ru(ahsH)(PPh3)2Cl], the tridentate ahsH2− binds to the metal ion via the deprotonated amide O, the imine N and the phenolate O atoms. In the electronic spectra, the green [Ru(HahsR)(PPh3)2Cl2] and brown [Ru(ahsR)(PPh3)2Cl] complexes display several absorptions in the ranges 385–283 and 457–269 nm, respectively. Both complexes are low-spin and display rhombic EPR spectra in frozen solutions. Both types of complexes are redox active and display a quasi-reversible ruthenium(III) to ruthenium(II) reduction which is sensitive to the polar effect of the substituent on the chelating ligand. The reduction potentials are in the ranges −0.21 to −0.12 and −0.42 to −0.21 V (versus Ag/AgCl) for [Ru(HahsR)(PPh3)2Cl2] and [Ru(ahsR)(PPh3)2Cl], respectively.  相似文献   

4.
N,N′-bis(3,5-dichlorosalicylidene)-2-hydroxy-1,3-diamino-2-propan (C17H14Cl4N2O3) was synthesized and its crystal structure determined. It crystallizes in the monoclinic space group, C2/c, with a=29.734(8), b=4.541(1), c=14.694(2) Å, β=115.85(2), R(F2)=0.048 for 1704 independent reflections. The title compound has a twofold axis passing through the central C9 atom. The intramolecular hydrogen bond occurs between the pairs of atoms N1 and O1 [2.648(5) Å] and the hydrogen atom is essentially being bonded to the nitrogen atom. There is no intermolecular proximity between molecules. Conformations of the title compound were investigated by semi-empirical quantum mechanical AM1 calculations. The optimized geometry of the molecular structure corresponding to the non-planar conformation is the most stable conformation in the theoretical calculations. The results strongly indicate that the minimum energy conformation is primarily determined by non-bonded steric interactions.  相似文献   

5.
Reactions of Li2[PdCl4] with N-(aroyl)-N′-(2,4-dimethoxybenzylidene)hydrazines (H2L = (4-R-C6H4)C(O)NHNCH(2,4-(CH3O)2C6H3)) in presence of PPh3 have provided cyclopalladated complexes having the general formula [PdL(PPh3)] (1, 2 and 3 where R = OCH3, CH3 and Cl, respectively) and a coordination complex trans-[Pd(HL)(PPh3)2Cl] (4 where R = NO2). The complexes have been characterized by elemental analysis, infrared, 1H NMR and electronic absorption spectroscopy. X-ray structures of all the complexes have been determined. In 1, 2 and 3, the C,N,O-donor dianionic ligand (L2−) forms two fused five-membered chelate rings at the metal centre. On the other hand, the monoanionic ligand (HL) acts as deprotonated amide N-donor in 4. The strong electron withdrawing effect of the nitro group on the aroyl fragment is possibly responsible for the monodentate amide N-coordinating behavior of HL in 4. The orientation of the 4-methoxy group in 1 is different than that in 2 and 3 due to intramolecular C-H?π interaction in the last two complexes. The structure of 4 shows an apical C-H?Pd interaction involving the azomethine (-CHN-) group of HL. In the crystal lattice of all the structures, various types of intermolecular non-covalent interactions are present. The self-assembly of the molecules of 1, 2 and 3 leads to two-dimensional networks. The same network observed for 2 and 3 reflects the interchangeability of the chloro and methyl groups due to their similar volumes. In the case of 4, the complex and the water molecules present in the crystal lattice form parallel homo-chiral helices and finally interhelical interactions lead to a three-dimensional network.  相似文献   

6.
N-2-(4-picolyl)-N′-2-chlorophenylthiourea, 4PicTu2Cl, monoclinic, P21/c, a=10.068(5), b=11.715(2), β=96.88(4)°, and Z=4; N-2-(6-picolyl)-N′-2-chlorophenylthiourea, 6PicTu2Cl, triclinic, P-1, a=7.4250(8), b=7.5690(16), c=12.664(3) Å, =105.706(17), β=103.181(13), γ=90.063(13)°, V=665.6(2) Å3 and Z=2 and N-2-(6-picolyl)-N′-2-bromophenylthiourea, 6PicTu2Br, triclinic, P-1, a=7.512(4), b=7.535(6), c=12.575(4) Å, a=103.14(3), β=105.67(3), γ=90.28(4)°, V=665.7(2) Å3 and Z=2. The intramolecular hydrogen bonding between N′H and the pyridine nitrogen and intermolecular hydrogen bonding involving the thione sulfur and the NH hydrogen, as well as the planarity of the molecules, are affected by the position of the methyl substituent on the pyridine ring. The enthalpies of fusion and melting points of these thioureas are also affected. 1H NMR studies in CDCl3 show the NH′ hydrogen resonance considerably downfield from other resonances in their spectra.  相似文献   

7.
Structures of the following compounds have been obtained: N-(2-pyridyl)-N′-2-thiomethoxyphenylthiourea, PyTu2SMe, monoclinic, P21/c, a=11.905(3), b=4.7660(8), c=23,532(6) Å, β=95.993(8)°, V=1327.9(5) Å3 and Z=4; N-2-(3-picolyl)-N′-2-thiomethoxyphenyl-thiourea, 3PicTu2SeMe, monoclinic, C2/c, a=22.870(5), b=7.564(1), c=16.941(4) Å, β=98.300(6)°, V=2899.9(9) Å3 and Z=8; N-2-(4-picolyl)-N′-2-thiomethoxyphenylthiourea, 4PicTu2SMe, monoclinic P21/a, a=9.44(5), b=18.18(7), c=8.376(12) Å, β=91.62(5)°, V=1437(1) Å3 and Z=4; N-2-(5-picolyl)-N′-2-thiomethoxyphenylthiourea, 5PicTu2SMe, monoclinic, C2/c, a=21.807(2), b=7.5940(9), c=17.500(2) Å, β=93.267(6)°, V=2893.3(5) Å3 and Z=8; N-2-(6-picolyl)-N′-2-thiomethoxyphenylthiourea, 6PicTu2SMe, monoclinic, P21/c, a=8.499(4), b=7.819(2), c=22.291(8) Å, β=90.73(3)°, V=1481.2(9) Å3 and Z=4 and N-2-(4,6-lutidyl)-N′-2-thiomethoxyphenyl-thiourea, 4,6LutTu2SMe, monoclinic, P21/c, a=11.621(1), b=9.324(1), c=14.604(1) Å, β=96.378(4)°, V=1572.4(2) Å3 and Z=4. Comparisons with other N-2-pyridyl-N′-arylthioureas having substituents in the 2-position of the aryl ring are included.  相似文献   

8.
Cyclopalladated complexes with the Schiff base N-(benzoyl)-N-(2,4-dimethoxybenzylidene)hydrazine (H2L, 1) have been described. The reaction of 1 with Li2[PdCl4] in methanol yields the complex [Pd(HL)Cl] (2). [Pd(HL)(CH3CN)Cl] (3) has been prepared by dissolving 2 in acetonitrile. In methanol-acetonitrile mixture, treatment of 2 with two mole equivalents of PPh3 produces [PdL(PPh3)] (4) and that with one mole equivalent of PPh3 produces [Pd(HL)(PPh3)Cl] (5). Crystallization of 2 from dmso-d6 results into isolation of [Pd(HL)((CD3)2SO)Cl] (6). In 2, the monoanionic ligand (HL) is C,N,O-donor and the Cl-atom is trans to the azomethine N-atom. In 3, 5 and 6, HL is C,N-donor and the Cl-atom is trans to the metallated C-atom. The remaining fourth coordination site is occupied by the N-atom of CH3CN, the P-atom of PPh3 and the S-atom of (CD3)2SO in 3, 5 and 6, respectively. Thus on dissolution in acetonitrile and dmso and in reaction with stoichiometric PPh3 the incoming ligand imposes a rearrangement of the coordinating atoms on the palladium centre. On the other hand, in presence of excess PPh3 deprotonation of the amide functionality in 2 occurs and the Cl-atom is replaced by the P-atom of PPh3 to form 4. Here the dianionic ligand (L2−) remains C,N,O-donor as in 2. The compounds have been characterized with the help of elemental analysis (C, H, N), infrared, 1H NMR and electronic absorption spectroscopy. Molecular structures of 3, 4, and 6 have been determined by X-ray crystallography.  相似文献   

9.
The reactions of Mo2(O2CCH3)4 with different equivalents of N,N′-bis(pyrimidine-2-yl)formamidine (HL1) and N-(2-pyrimidinyl)formamide (HL2) afforded dimolybdenum complexes of the types Mo2(O2CCH3)(L1)2(L2) (1) trans-Mo2(L1)2(L2)2 (2) cis-Mo2(L1)2(L2)2 (3) and Mo2(L2)4 (4). Their UV–Vis and NMR spectra have been recorded and their structures determined by X-ray crystallography. Complexes 2 and 3 establish the first pair of trans and cis forms of dimolybdenum complexes containing formamidinate ligands. The L1 ligands in 13 are bridged to the metal centers through two central amine nitrogen atoms, while the L2 ligands in 14 are bridged to the metal centers via one pyrimidyl nitrogen atom and the amine nitrogen atom. The Mo–Mo distances of complexes 1 [2.0951(17) Å], 2 [2.103(1) Å] and 3 [2.1017(3) Å], which contain both Mo?N and Mo?O axial interactions, are slightly longer than those of complex 4 [2.0826(12)–2.0866(10) Å] which has only Mo?O interactions.  相似文献   

10.
Thermal substitution reaction of Cr(CO)42:2-1,5-cyclooctadiene), Mo(CO)42:2-norbornadiene), and W(CO)52-bis(trimethylsilyl)ethyne) with N,N′-bis(ferrocenylmethylene)ethylenediamine (bfeda) yields M(CO)4(bfeda) complexes which could be isolated from the reaction solution and characterized by elemental analysis, MS, IR, and NMR spectroscopy. In the case of tungsten, W(CO)5(bfeda) is formed as intermediate and then undergoes the ring closure reaction yielding the ultimate product W(CO)4(bfeda). The electrochemical behavior of the M(CO)4(bfeda) complexes was studied by using cyclic voltammetry (CV) and differential pulse voltammetry (DPV) in dichloromethane with tetrabutylammonium tetrafluoroborate as electrolyte. Constant potential electrolysis of the complexes was performed successively at their peak potentials at 0 °C in their CH2Cl2 solution and the electrolysis was followed by in situ recording the electronic absorption spectra in every 5 mC. In the electrolysis of Cr(CO)4(bfeda), the central Cr(0) is oxidized first and electrolysis continues with oxidations of two ferrocenyl groups until the end of totally three moles of electron passage per mole of complex. In the electrolysis of Mo(CO)4(bfeda) and W(CO)4(bfeda) the first oxidation occurs on the central atom forming a short-lived species which undergoes an intramolecular one-electron transfer and is reduced back to M(0) while one of the ferrocene units is oxidized to the ferrocenium cation at the same time. This indicates that the electron is transferred from iron to the central metal atom.  相似文献   

11.
A series of novel triphenylamine-containing aromatic poly(amine-amide)s were prepared from the dicarboxylic acid, N,N′-bis(4-carboxyphenyl)-N,N′-diphenyl-1,4-phenylenediamine, and various diamines by direct phosphorylation polycondensation. All the poly(amine-amide)s were amorphous, soluble in a variety of organic solvents, and could be solution cast into transparent, tough, and flexible films with good mechanical properties. They had useful levels of thermal stability associated with relatively high glass-transition temperatures (195-280 °C). These polymers exhibited strong UV-Vis absorption bands at 330-346 nm and their photoluminescence showed maximum bands around 516-535 nm in NMP solution. The hole-transporting and electrochromic properties are examined by electrochemical and spectroelectrochemical methods. Cyclic voltammograms of the poly(amine-amide)s prepared by casting polymer solution onto an indium-tin oxide (ITO)-coated glass substrate exhibited two reversible oxidative redox couples at potential 0.73-0.78 V and 1.12-1.18 V, respectively vs Ag/AgCl in acetonitrile solution. All the poly(amine-amide)s exhibited excellent reversibility of electrochromic characteristics by continuous ten cyclic scans between 0.0 and 1.40 V, with a color change from original pale yellowish neutral form to the green and then to blue oxidized forms.  相似文献   

12.
A series of N-(1,2,4-triazole-4-yl)-N′-(fluorine-containing-phenyl)carbamimidothioates 5a-i were synthesized by reacting 4-amine-1,2,4-trizaole with corresponding aryl isothiocyanates in ethanol at room temperature and, in a subsequent step, with methyl iodide. The antifungal activities of the title compounds against the fungi Rhizoctonia solan and Pyricularia orizae were screened.  相似文献   

13.
The syntheses of the compounds [M(Cp)(aeaz)(az)](OTf)2 (4, 5) (M = Rh(III), Ir(III); aeaz = C2H4NC2H4NH2, az = C2H4NH (3)) containing cationic N-(2-aminoethyl)aziridine-N,N′ chelate complexes are described. The bis-aziridine complexes [MCl(Cp)(az)2]Cl (M = Rh (1), M = Ir (2)) react with an excess of the aziridine (az) in the presence of AgO3SCF3 (=AgOTf) via AgCl precipitation and az addition followed by a metal-mediated coupling reaction, to give the compounds [M(Cp)(aeaz)(az)](OTf)2 (4, 5). The new aeaz ligand is formally the dimerisation product of az. Using the same reaction conditions with the analogous, but weaker Lewis acidic ruthenium(II) complex [RuCl(C6Me6)(az)2]Cl (6) an anion exchange reaction yielding [RuCl(C6Me6)(az)2]OTf (8) is observed. After purification, all compounds are fully characterized using IR, FAB-MS, 1H and 13C NMR spectroscopy. The single crystal X-ray structure analysis reveals a distorted octahedral geometry for all complexes.  相似文献   

14.
A new thiourea derivative, N-(biphenyl-2-thiocarbamoyl)-4-phenylcarboxamide, is synthesized and characterized by elemental analysis, FTIR, NMR and the single crystal X-ray diffraction study. The title compound crystallizes with two molecules in the asymmetric unit. The dihedral angle between the two aromatic rings in the biphenyl unit is 47.9(2) and 56.52(19)°, respectively, for the two molecules in the asymmetric unit. The molecular conformation is stabilized by intramolecular NH?O hydrogen bond. The crystal packing shows that the molecules form centrosymmetric dimers connected by NH?S hydrogen bonds. The vibrational properties have been studied by FTIR and FT-Raman spectroscopy along with quantum chemical calculations at the B3LYP/6-311 + G* level of approximation. The main normal modes related with the thioamide bands are discussed.  相似文献   

15.
The syntheses and crystal structures of four new uranyl complexes with [O,N,O,N′]-type ligands are described. The reaction between uranyl nitrate hexahydrate and the phenolic ligand [(N,N-bis(2-hydroxy-3,5-dimethylbenzyl)-N′,N′-dimethylethylenediamine)], H2L1 in a 1:2 molar ratio (M to L), yields a uranyl complex with the formula [UO2(HL1)(NO3)] · CH3CN (1). In the presence of a base (triethylamine, one mole per ligand mole) with the same molar ratio, the uranyl complex [UO2(HL1)2] (2) is formed. The reaction between uranyl nitrate hexahydrate and the ligand [(N,N-bis(2-hydroxy-3,5-di-t-butylbenzyl)-N′,N′-dimethylethylenediamine)], H2L2, yields a uranyl complex with the formula [UO2(HL2)(NO3)] · 2CH3CN (3) and the ligand [N-(2-pyridylmethyl)-N,N-bis(2-hydroxy-3,5-dimethylbenzyl)amine], H2L3, in the presence of a base yields a uranyl complex with the formula [UO2(HL3)2] · 2CH3CN (4). The molecular structures of 14 were verified by X-ray crystallography. The complexes 14 are zwitter ions with a neutral net charge. Compounds 1 and 3 are rare neutral mononuclear [UO2(HLn)(NO3)] complexes with the nitrate bonded in η2-fashion to the uranyl ion. Furthermore, the ability of the ligands H2L1–H2L4 to extract the uranyl ion from water to dichloromethane, and the selectivity of extraction with ligands H2L1, H3L5 (N,N-bis(2-hydroxy-3,5-dimethylbenzyl)-3-amino-1-propanol), H2L6 · HCl (N,N-bis(2-hydroxy-5-tert-butyl-3-methylbenzyl)-1-aminobutane · HCl) and H3L7 · HCl (N,N-bis(2-hydroxy-5-tert-butyl-3-methylbenzyl)-6-amino-1-hexanol · HCl) under varied chemical conditions were studied. As a result, the most efficient and selective ligand for uranyl ion extraction proved to be H3L7 · HCl.  相似文献   

16.
Two structurally different complexes, [Cu2(2-NO2Bz)4(denia)1]n (1) and [Cu(2-NO2Bz)2(denia)2(H2O)2] (2), were prepared from the same reaction (where 2-NO2Bz = 2-nitrobenzoate, denia = N,N-diethylnicotinamide) and they are reported together with [Cu2(2-NO2Bz)4(DMF)2] (3) (DMF = N,N-dimethylformamide). The compounds under study were characterized by elemental analysis, electronic, IR and EPR spectra, magnetic measurements over the temperature range of 1.8–300 K and X-ray analysis. The molecular structure of (1) is polymeric, (2) is monomeric and (3) is dimeric. In the polymeric chain of (1), the denia molecules serve as bridges between dimeric Cu2(2-NO2bz)4 units. Each Cu(II) atom has a square-pyramidal arrangement with different chromophores, Cu1O4O′ and Cu2O4N. The Cu–Cu distances are 2.699(1) Å in the dimeric unit and 7.980(3) Å between the dimeric units. In (2) the Cu(II) atom has a tetragonal-bipyramidal environment CuO2N2O′2. In (3) two Cu(II) atoms are bridged by four carboxylate groups of four 2-NO2bz anions in a synsyn arrangement which create a square base about each Cu(II) atom and an apical position is occupied by the O atom of a DMF molecule (CuO4O′). The Cu–Cu distance of 2.633(1) Å is somewhat shorter than in (1). Spectral and magnetic data of the complexes are discussed with their structures.  相似文献   

17.
The syntheses and structures of a series of metal complexes, namely Cu2Cl4(L1)(DMSO)2·2DMSO (L1 = N,N′-bis(2-pyridinyl)-1,4-benzenedicarboxamide), 1; {[Cu(L2)1.5(DMF)2][ClO4]2·3DMF} (L2 = N,N′-bis(3-pyridinyl)-1,4-benzenedicarboxamide), 2; {[Cd(NO3)2(L3)]·2DMF} (L3 = N,N′-bis-(2-pyrimidinyl)-1,4-benzenedicarboxamide), 3; {[HgBr2(L3)]·H2O}, 4, and {[Na(L3)2][Hg2X5]·2DMF} (X = Br, 5; I, 6) are reported. All the complexes have been characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. Complex 1 is dinuclear and the molecules are interlinked through S?S interactions. In 2, the Cu(II) ions are linked through the L2 ligands to form 1-D ladder-like chains with 60-membered metallocycles, whereas complexes 3 and 4 form 1-D zigzag chains. In complexes 5 and 6, the Na(I) ions are linked by the L3 ligands to form 2-D layer structures in which the [Hg2X5] anions are in the cavities. The L2 ligand acts only as a bridging ligand, while L1 and L3 show both chelating and bridging bonding modes. The L1 ligand in 1 adopts a trans-anti conformation and the L2 ligand in 2 adopts both the cis-syn and trans-anti conformations, whereas the L3 ligands in 36 adopt the trans conformation.  相似文献   

18.
19.
The Schiff base compound, N,N′-bis(trifluoromethylbenzylidene)ethylenediamine (C18H14F6N2) (1), CF3C6H4CHNCH2CH2NCHC6H4CF3 has been synthesized by adding a solution of ethylenediammine (en), 0.1 mmol in chloroform to 4-(trifluoromethyl)-benzaldehyde, CF3C6H4CHO (0.2 mmol) and the product was crystallized in ethanol with the mp, 109.2 °C and 75% yield. The crystal structure was investigated by a single-crystal X-ray diffraction study at 150 K. The compound crystallizes in monoclinic space group, P21/c with a = 9.295(3), b = 5.976(5), c = 15.204(9) Å and α = 90°, β = 96.56(5)° and γ = 90°. The crystal structure is stabilized by intermolecular CH · · · F hydrogen bonds. The asymmetric unit contains only one-half of the molecule related to the center of symmetry coinciding with C(1)-C(1′) and as a whole, the title molecule is in the staggered conformation. The phenyl rings and the CN imine bonds are co-planar. The infrared spectrum showed a sharp peak at 1640 cm−1 which is typical of the conjugated CN stretching and strong peaks at 800-1400 cm−1 regions are due to the C-C and C-H stretching modes. Electronic absorption spectra exhibits strong absorption in the UV region (240 nm wavelength) which have been ascribed to , and electronic transitions. The 1H NMR spectra showed three distinct peaks at 2.5, 7.8 and 8.5 ppm which are assigned based on the splitting of resonance signals and are clearly confirmed by the X-ray molecular structure. The aromatic protons appear at about 7.8 ppm and the imine protons at 8.5 ppm. The sharp singlet at about 3.95 ppm is assigned to the CH2-CH2 protons. Mass spectra of the titled compound showed the molecular ion peak at m/e 372 (M+), and fragments at m/e 353 (M-F), 342 (M-2F), 200 (M-CF3C6H4CHN), 186 (M-CF3C6H4CHNCH2).  相似文献   

20.
The reaction of boron heterocycles 1 and 2 with n-butyl lithium and alkyl halides led to (N→B) phenyl[N-alky-N-(2-alkyl)aminodiacetate-O,O′,N]boranes 36(ab), 7(b) and 9(b), where alkyl can be in exo and/or endo position, and phenyl[N-alkyl-N-(2-alkyl)aminodiacetate-O,O′,N]boranes 7(c) and 8(c) isomers, which do not display the intramolecular N→B coordination bond. The existence of steric interactions between N-benzyl and the alkyl group at 2 position was indicated by 1H and 13C NMR, while, the δ(11B) values confirm the tetrahedral and trigonal environment of the 11B nucleus in these compounds. Moreover, the compounds were characterized by COSY, HETCOR and homonuclear proton decoupling experiment. The study of the intramolecular N→B coordination by dynamic NMR afforded a ΔG‡ value of 81.09 kJ/mol for compound 6(b).  相似文献   

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