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1.
Synthesis, structures and some reactions of Ru(CCCCFc)(PP)Cp (PP = dppm, dppe) and related compounds
Michael I. Bruce Frédéric de Montigny Martyn Jevric Brian W. Skelton Allan H. White 《Journal of organometallic chemistry》2004,689(18):2860-2871
The compounds Ru(CCCCFc)(PP)Cp [PP = dppe (1), dppm (2)], have been obtained from reactions between RuCl(PP)Cp and FcCCCCSiMe3 in the presence of KF (1) or HCCCCFc and K[PF6] (2), both with added dbu. The dppe complex reacts with Co2(CO)6(L2) [L2 = (CO)2, dppm] to give 3, 4 in which the Co2(CO)4(L2) group is attached to the outer CC triple bond. The PPh3 analogue of 3 (5) has also been characterised. In contrast, tetracyanoethene reacts to give two isomeric complexes 6 and 7, in which the cyano-olefin has added to either CC triple bond. The reaction of RuCl(dppe)Cp with HCCCCFc, carried out in a thf/NEt3 mixture in the presence of Na[BPh4], gave [Ru{CCC(NEt3)CHFc}(dppe)Cp]BPh4 (8), probably formed by addition of the amine to an (unobserved) intermediate butatrienylidene [Ru(CCCCHFc)(dppe)Cp]+. The reaction of I2 with 8 proceeds via an unusual migration of the alkynyl group to the Cp ring to give [RuI(dppe){η-C5H4CCC(NEt3)CHFc}]I3 (9). Single-crystal X-ray structural determinations of 1, 2 and 4-9 are reported. 相似文献
2.
Shuji YasuikeSatoru Okajima Kentaro YamaguchiHiroko Seki Jyoji Kurita 《Tetrahedron》2003,59(27):4959-4966
Racemic 2,2′-bis[diarylstibano]-1,1′-binaphthyls [(±)-BINASbs] and 2,2′-bis[di(p-tolyl)bismuthano]-1,1′-binaphthyl [(±)-BINABi], which are the antimony and bismuth congeners of BINAP, have been prepared from 2,2′-dibromo-1,1′-binaphthyl (DBBN) via 2,2′-dilithio-1,1′-binaphthyl intermediate by treatment with the appropriate metal halides [(p-Tol)2SbBr, Ph2SbBr and (p-Tol)2BiCl]. The optical resolution of the (±)-BINASbs could be achieved via the separation of a mixture of the diastereomeric Pd-complexes derived from the reaction of (±)-BINASbs with di-μ-chlorobis{(S)-2-[1-(dimethylamino)-ethyl]phenyl-C1,N}dipalladium(II). Optically active (R)-BINASb and (R)-BINABi could be also obtained from optically active (R)-DBBN by the same procedure. The enantiopure BINASbs have been shown to be effective chiral ligands for the rhodium-catalyzed asymmetric hydrosilylation of ketones. 相似文献
3.
Sheng-Huei Hsiao Chin-Ping Yang Sheng-Wen Wang Ming-Hung Chuang 《Journal of polymer science. Part A, Polymer chemistry》1999,37(18):3575-3583
1,1-Bis[4-(4-carboxyphenoxy)phenyl]cyclohexane (III) and 1,1-bis[4-(4-aminophenoxy)phenyl]cyclohexane (V) were prepared in two main steps starting from the aromatic nucleophilic substitution of p-fluorobenzonitrile and p-chloronitrobenzene, respectively, with 1,1-bis(4-hydroxyphenyl)cyclohexane in the presence of potassium carbonate in N,N-dimethylformamide (DMF). Using triphenyl phosphite and pyridine as condensing agents, two series of polyamides with cyclohexylidene cardo groups were directly polycondensated from dicarboxylic acid III with various aromatic diamines or from diamine V with various aromatic dicarboxylic acids in an N-methyl-2-pyrrolidone (NMP) solution containing dissolved calcium chloride. The polyamides exhibited inherent viscosities in the range of 0.45 to 1.78 dL/g. Almost all of the polymers were readily soluble in polar aprotic solvents such as NMP and N,N-dimethylacetamide (DMAc) and could afford transparent, flexible, and tough films by solution casting. The glass transition temperatures (Tg) of these aromatic polyamides were in the range of 180–243°C by DSC, and the 10% weight loss temperatures in nitrogen and air were all above 450°C. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 3575–3583, 1999 相似文献
4.
采用乙醚蒸汽扩散法,由四氟合硼酸四乙腈合铜(Ⅰ)、4,4′-联吡啶、二(2-二苯基膦基)苯基醚或者三苯基膦的反应后的二氯甲烷和乙腈混合溶液中,晶化出[Cu2(4,4′-bipy)(POP)2(CH3CN)2(C2H5O)2](BF4)2 (1)和[Cu2(4,4′-bipy)(PPh3)4(CH3CN)2](BF4)2 (2)两种配合物。对它们进行了元素分析和X射线衍射单晶结构表征,同时测定了UV-Vis光谱及相应的激发态寿命。配合物1和2展示了较好的光物理特性,在275 nm紫外光的激发下,固体粉末样品的最大发射峰位分别位于527和483 nm,这归因于金属干扰的配体内部跃迁。 相似文献
5.
6.
Jean-Luc Montchamp 《Journal of organometallic chemistry》2005,690(10):2388-2406
This account summarizes the research conducted in our laboratory over the past five years. New methodologies were devised for the formation of P-C bonds with a focus on the reactions of hypophosphorous acid derivatives. Three types of reactions have been developed: palladium-catalyzed cross-coupling, room-temperature radical addition, and palladium-catalyzed addition. Our results are summarized in each of these areas and include some of our most recent data. (1) Our palladium-catalyzed cross-coupling has been extended to the direct coupling of alkyl phosphinates with a variety of aryl, heteroaryl, and even alkenyl electrophiles. (2) The addition of sodium hypophosphite under radical conditions is extended from alkenes to alkynes. (3) The catalytic addition of hypophosphorous compounds using palladium catalysts (hydrophosphinylation) is also discussed. 相似文献
7.
Nanoparticles of (R)-1,1′-bi-2-naphthol dibenzoate (R-BND) ranging from 40 to 170 nm were prepared by using the reprecipitation method. The nanoparticles exhibit size-dependent exciton chirality, where the coupling potential V12 of 1Bb transitions increases as nanoparticles grow and simultaneously the exciton chirality peaks exhibit the bathochromic shift. Such size-dependent optical properties can be attributed to the lattice hardening with increased particle size, which leads to a decreased dihedral angel θ between the two naphthyl planes in a R-BND molecule. 相似文献
8.
Chin-Ping Yang Ruei-Shin Chen Chi-Chi Huang 《Journal of polymer science. Part A, Polymer chemistry》1999,37(14):2421-2428
Alternate poly(amide-imide) [P(A-alt-I)] was synthesized from two aromatic diamines and trimellitic anhydride (TMA). When the diamine was 2,2-bis[4-(3-aminophenoxy)phenyl]sulfone (BAPS), the resulted P(A-alt-I) was found to be of light color. Specifically, when BAPS was located between two amide groups in the P(A-alt-I) chain, the P(A-alt-I) was almost colorless. A series of P(A-alt-I)s (Series III) containing BAPS was synthesized through direct polycondensation of an aromatic dicarboxylic acid prepared from various aromatic diamines and TMA, as well as BAPS. Polymers of Series III were much lighter in color than those of the isomeric series (BAPS was located between two imide group). The series of P(A-alt-I)s III had inherent viscosities ranging 0.69–1.35 dL/g and good solubility in various solvents. The tensile strengths, elongations to break, and initial moduli of the films were 72–107 MPa, 7–12% and 1.93–2.39 GPa, respectively, and most of the films had no yielding. Polymers of Series III had glass transition temperatures 210–272°C and 10% weight loss temperatures in nitrogen 518–545°C, indicating excellent thermal stability. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 2421–2428, 1999 相似文献
9.
S. G. Peeran G. Hanumantha Reddy 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4):9-22
Abstract The synthesis of (E)- and (Z)-1.2-bis(p-fluorophenylsulphenyl)stilbenes (2a and 2b) and 1,2-bis(p-fluorophenylsulphonyl)stilbenes (3a and 3b) was carried out and their configurations were consistent with their stereospecific synthesis. The isomeric 1,1-bis(p-fluorophenylsulphenyl)- and 1,1-bis(p-fluorophenylsulphonyl)-2,2-bis(phenyl)ethylenes (8 and 9) were also synthesised and configurations were established by degradative oxidation. Mass spectral rearrangements of all these compounds were examined. Mass spectra of 1,1-bis-sulphide and 1,1-bis-sulphone bears close relationship with those of (E)- and (Z)-isomeric counterparts. Smiles-type rearrangement observed in 1,2-bis-sulphides was absent in 1,2-bis-sulphones. McLafferty-type rearrangement involving hydrogen migration, from aryl group was noticed in both bis-sulphides and bis-sulphones. Vinyl migration to the sulphone oxygen predominates over aryl migration in three isomeric bis-sulphones. 相似文献
10.
New photochromic title compounds 1, 2, and 3 have been prepared starting from 4-methylphthalic anhydride. Compounds 3a and 3b are a pair of enantiomers and were obtained as a racemic mixture (numbered as 3). Compounds 1, 2, and 3 were successfully separated from the isomeric mixture product through fractional crystallization, and their structures are confirmed by X-ray crystallographic analysis. UV-vis absorption and photochromic properties of 1, 2, and 3 have also been investigated. Results reveal that the substituents, even like the simple methyl, on the benzene rings of biindenylidenedione could considerably affect the photochromic property, as well as other properties of this kind of compounds. 相似文献
11.
Der-Jang Liaw Been-Yang Liaw 《Journal of polymer science. Part A, Polymer chemistry》1999,37(15):2791-2794
A new diamine, 2,2-bis[4-(4-aminophenoxy)phenyl]norbornane (BAPN), containing both ether and norbornane cardo groups, was synthesized in three steps started from norcamphor. A series of cardo polyamides were obtained by the direct polycondensation of BAPN and various aromatic dicarboxylic acids in N-methyl-2-pyrrolidinone (NMP) using triphenyl phosphite and pyridine as condensing agents. Polyamides had inherent viscosities in the range of 0.82–1.58 dL g−1, and were readily soluble in polar aprotic solvents such as NMP, N,N-dimethylacetamide (DMAc) and N,N-dimethylformamide and dimethyl sulfoxide. These polymers were cast in DMAc solution into transparent, flexible, and tough films that were further characterized by X-ray and mechanical analysis. All the polymers were amorphous, and the polyamide films had a tensile strength range of 71–89 MPa, an elongation at break range of 5–9%, and a tensile modulus range of 2.0–2.3 GPa. Polyamides showed glass transition temperatures in the range of 256–296°C as measured by DSC and thermogravimetric analysis indicated no weight loss below 450°C in nitrogen and air atmosphere. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 2791–2794, 1999 相似文献
12.
Shin-ichi Takekuma Masanori Hirosawa Masato Sasaki Hideko Takekuma 《Tetrahedron》2006,62(15):3732-3738
Reactions of the title ethylene derivatives, (E)-1,2-di(3-guaiazulenyl)ethylene (1) and 2-(3-guaiazulenyl)-1,1-bis(4-methoxyphenyl)ethylene (2), with a 2 M amount of TCNE in benzene at 25 °C for 24 h under argon give new cycloaddition compounds, 1,1,2,2,11,11,12,12-octacyano-3-(3-guaiazulenyl)-8-isopropyl-5,10-dimethyl-1,2,3,6,9,10a-hexahydro-6,9-ethanobenz[a]azulene (3) from 1 and 1,1,2,2,11,11,12,12-octacyano-8-isopropyl-3,3-bis(4-methoxyphenyl)-5,10-dimethyl-1,2,3,6,9,10a-hexahydro-6,9-ethanobenz[a]-azulene (4) from 2, respectively, in 66 and 87% isolated yields. Comparative studies on the above reactions as well as the spectroscopic properties of the unique products 3 and 4, possessing interesting molecular structures, are reported and, further, a plausible reaction pathway for the formation of these products is described. 相似文献
13.
H. Hong 《Journal of organometallic chemistry》2004,689(1):58-64
Cyclic 1,2-diphenylenediboranes containing a doubly hydrogen-bridged structure, including 1,2-(2,2′biphenylylene)diborane(I) and 1,2-(2,2′biphenylylene)-1,2-diethyldiborane (II), are conveniently prepared by treating 9-chloro-9-borafluorene with NaBH4 and Na(Et)3BH, respectively. The reaction mechanism involves an initial Cl-H exchange to form 9-borafluorene containing a reactive 5-member ring diarylborane moiety, which subsequently engages in a facile ring expansion with the in situ formed B-H containing residue (BH3 or HBEt2) to result in cyclic 1,2-diphenylenediboranes compounds. The doubly hydrogen-bridged structure shows good thermal stability up to 50 °C. Upon thermal cleavage at higher temperature, all free B-H groups become very reactive involving hydroboration with α-olefin. The complexization study also reveals that this intradiborane moiety forms a 1:2 complex with a strong base, such as pyridine. 相似文献
14.
Jugal Kishore Puri Raghubir Singh Raj Pal Sharma Edwin Kroke 《Journal of organometallic chemistry》2011,696(7):1341-1348
The present work aims at the synthesis of various novel silatranes bearing substituted urea functionality. Nucleophilic addition of various amines (morpholine, aniline, ethylenediamine and 3-aminopropyltriethoxysilane) to 3-isocyanatopropyltriethoxysilane resulted in the four triethoxysilanes; N-[3-(triethoxysilyl)propyl]morpholine-4-carboxylic acid amide (1), 1-[3-(triethoxysilyl)propyl]-3-phenylurea (2), 1,2-bis{N′-[3-(triethoxysilyl)propyl]ureido}-ethane (3) and N-[3-(triethoxysilyl)propyl]-N′-[3-(triethoxysilyl)propyl]urea (4), respectively. In the presence of a base the resulting silanes undergo transesterification reaction with triethanolamine, thus forming the corresponding silatranes, N-(3-silatranylpropyl)morpholine-4-carboxylic acid amide (5), 1-(3-silatranylpropyl)-3-phenylurea (6), 1,2-Bis[N′-(3-silatranylpropyl)ureido]-ethane (7) and N-(3-silatranylpropyl)-N′-(3-silatranylpropyl)urea (8), respectively. Among these are four novel compounds (5-8), which were characterized by elemental analysis, IR, multinuclear (1H, 13C and 29Si) NMR and mass spectroscopy. Structures of compounds 5 and 6 were deduced by X-ray crystallography. Single crystal X-ray studies revealed distorted trigonal bipyramidal coordination about Si in 5 and 6 with Si-N bond distance of 2.121(1) Å and 2.189(2) Å, respectively. 相似文献
15.
Nader Noroozi Pesyan Vali GolsanamlooShahnaz Ganbari Ertan ?ahin 《Tetrahedron letters》2012,53(32):4096-4099
A simple and efficient unusual coupling reaction of 9-(2-hydroxy-4,4-dimethyl-6-oxocyclohex-1-en-1-yl)-3,3-dimethyl-2,3,4,9-tetrahydro-1H-xanthen-1-one and its derivatives was accomplished in the presence of Mn2+, Cu2+, Cd2+, Hg2+, Fe3, or La3+. The structure elucidation was accomplished by IR, 1H NMR, 13C NMR, X-ray crystallography, UV-Visible and elemental analysis. A reaction mechanism is proposed. 相似文献
16.
Chin-Ping Yang Sheng-Huei Hsiao Jiun-Hung Lin 《Journal of polymer science. Part A, Polymer chemistry》1993,31(12):2995-3002
A dicarboxylic acid ( 1 ) bearing two pre-formed imide rings, was prepared from the condensation of 2,2-bis[4-(4-aminophenoxy)phenyl]propane and trimellitic anhydride. A new family of poly(amide-imide)s having inherent viscosities of 0.53–1.68 dL/g was prepared by the triphenyl phosphite activated polycondensation from the diimide—diacid I with various aromatic diamines in a medium consisting of N-methyl-2-pyrolidone (NMP), pyridine, and calcium chloride. Most of the resulting polymers showed an amorphous nature and were readily soluble in polar solvents such as NMP and N,N-dimethylacetamide. All the soluble poly(amide-imide)s afforded transparent, flexible, and tough films. The glass transition temperatures of these poly(amide-imide)s were in the range of 237–293°C and the 10% weight loss temperatures were above 508°C in nitrogen. © 1993 John Wiley & Sons, Inc. 相似文献
17.
Hyung Joon Jeon 《Tetrahedron letters》2010,51(48):6243-6245
5,5′-Dibromo-2,2′-dipyridylacetylene was prepared from 2,5-dibromopyridine and (trimethylsilyl)acetylene via the new one-pot synthesis approach using a regioselective palladium-catalyzed coupling reaction with a 60% yield. Several protocols of lithium-halogen exchange were then attempted to synthesize 6,6′-(1,2-ethynediyl)bis[3-pyridylboronic acid] from 5,5′-dibromo-2,2′-dipyridylacetylene. The former was successfully obtained with a 54% yield by a reverse addition method using toluene and THF and it showed potential as a useful building block for cross-coupling reactions in the formation of carbon-carbon bonds. 相似文献
18.
F. Z. Galin N. M. andriyashina T. V. Le Yu. V. Tomilov V. V. Shereshovets 《Russian Chemical Bulletin》1999,48(8):1591-1592
The decomposition of 2-[4-(2-chloro-1,1-dimethylethyl)phenyl]propan-2-yl hydroperoxide in acetone catalyzed by H2SO4 affords 4-(2-chloro-1,1-dimethylethyl)phenol. The kinetics of this reaction at 56°C was studied.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1612–1613, August, 1999. 相似文献
19.
Gareth J. Rowlands Author Vitae 《Tetrahedron》2009,65(42):8603-1107
20.
A wide variety of monobrominated compounds 2a-l have been prepared in good yields from (E)-1-(2′-hydroxy-4′,6′-dimethoxyphenyl)-3-aryl-2-propen-1-ones (1a-l) through regioselective ring bromination using 1.5 equiv of bromodimethylsulfonium bromide (BDMS) at room temperature. Similarly, some of the 2′-hydroxychalcones can be converted directly into tribromides 3 or dibromides 4 by employing 4.0 equiv of BDMS under different reaction conditions which in turn can be transformed into 8-bromoflavones and 7-bromoaurones on treatment with 0.2 M ethanolic KOH solution. Mild reaction conditions, good yields and no chromatographic separation are some of the salient features of the present protocol. 相似文献