- Additive-freeN-methylation of amines with methanol over supported iridium catalyst
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An efficient and versatile zinc oxide-supported iridium (Ir/ZnO) catalyst was developed to catalyze the additive-freeN-methylation of amines with methanol. Mechanistic studies suggested that the high catalytic reactivity is rooted in the small sizes (1.4 nm) of Ir nanoparticles and the high ratio (93%) of oxidized iridium species (IrOx, Ir3+and Ir4+) on the catalyst. Moreover, the delicate cooperation between the IrOxand ZnO support also promoted its high reactivity. The selectivity of this catalyticN-methylation was controllable between dimethylation and monomethylation by carefully tuning the catalyst loading and reaction solvent. Specifically, neat methanol with high catalyst loading (2 mol% Ir) favored the formation ofN,N-dimethylated amine, while the mesitylene/methanol mixture with low catalyst loading (0.5 mol% Ir) was prone to producing mono-N-methylated amines. An environmentally benign continuous flow system with a recycled mode was also developed for the efficient production ofN-methylated amines. With optimal flow rates and amine concentrations, a variety ofN-methylamines were produced with good to excellent yields in this Ir/ZnO-based flow system, providing a starting point for the clean and efficient production ofN-methylamines with this cost-effective chemical process.
- Liu, Xiang,Loh, Teck-Peng,Qiang, Wenwen,Wang, Jing,Ye, Sen,Zhu, Longfei
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p. 3364 - 3375
(2021/06/06)
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- Method for realizing N-alkylation by using alcohols as carbon source under photocatalysis
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The invention discloses a method for realizing N-alkylation by using alcohols as a carbon source under photocatalysis, and belongs to the technical field of catalytic synthesis. Alcohol, a substrate raw material and a catalyst are placed in a reaction device, ultraviolet and/or visible light irradiation is carried out in an inert atmosphere, after the irradiation is finished, solid-liquid separation is carried out to remove the catalyst, and an N-alkylation product can be obtained through extraction, distillation and purification, wherein the substrate raw material comprises any one of an amine compound, an aromatic nitro compound or an aromatic nitrile compound, the alcohol comprises any one or more of soluble primary alcohols, and the catalyst is metal oxide/titanium dioxide or metal sulfide/titanium dioxide. The method is simple and easy to operate, can be used for efficient photocatalysis one-pot multi-step hydrogenation N-alkylation reaction, and is mild in reaction condition, high in chemical selectivity of N-alkylamine, good in catalyst stability and easy to recycle.
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Paragraph 0048-0056; 0058
(2021/03/13)
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- Novel hybrid conjugates with dual estrogen receptor α degradation and histone deacetylase inhibitory activities for breast cancer therapy
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Hormone therapy targeting estrogen receptors is widely used clinically for the treatment of breast cancer, such as tamoxifen, but most of them are partial agonists, which can cause serious side effects after long-term use. The use of selective estrogen receptor down-regulators (SERDs) may be an effective alternative to breast cancer therapy by directly degrading ERα protein to shut down ERα signaling. However, the solely clinically used SERD fulvestrant, is low orally bioavailable and requires intravenous injection, which severely limits its clinical application. On the other hand, double- or multi-target conjugates, which are able to synergize antitumor activity by different pathways, thus may enhance therapeutic effect in comparison with single targeted therapy. In this study, we designed and synthesized a series of novel dual-functional conjugates targeting both ERα degradation and histone deacetylase inhibiton by combining a privileged SERD skeleton 7-oxabicyclo[2.2.1]heptane sulfonamide (OBHSA) with a histone deacetylase inhibitor side chain. We found that substituents on both the sulfonamide nitrogen and phenyl group of OBHSA unit had significant effect on biological activities. Among them, conjugate 16i with N-methyl and naphthyl groups exhibited potent antiproliferative activity against MCF-7 cells, and excellent ERα degradation activity and HDACs inhibitory ability. A further molecular docking study indicated the interaction patterns of these conjugates with ERα, which may provide guidance to design novel SERDs or PROTAC-like SERDs for breast cancer therapy.
- Zhao, Chenxi,Tang, Chu,Li, Changhao,Ning, Wentao,Hu, Zhiye,Xin, Lilan,Zhou, Hai-Bing,Huang, Jian
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- Halogenated method of aromatic compound
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The invention belongs to the field of organic synthesis, and particularly relates to synthesis of aromatic halogens, in particular to arylamine. The invention discloses a synthesis method of a corresponding ortho-halogenated product from aromatic compounds such as carbazole and phenol. The method comprises the following steps: adding a metal sulfonate salt catalyst, aromatic amine, carbazole, phenol and other hydrogen - heteroatom-containing aromatic compound reaction substrates, a halogenation reagent and a reaction solvent at a specific reaction temperature. After the drying agent is dried, the yield of the reaction product and the nuclear magnetic characterization determining structure are determined by column chromatography. The reaction product yield is determined by gas chromatography. By adopting the method, under the cheap metal salt catalyst, a plurality of ortho-substituted brominated and chloro products can be obtained with moderate to excellent yield.
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Paragraph 0034-0037; 0227-0229; 0238
(2021/11/10)
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- N -Methylation of ortho -substituted aromatic amines with methanol catalyzed by 2-arylbenzo [d] oxazole NHC-Ir(iii) complexes
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Seven new chelated cyclometalated Ir complexes of ABON,P, ABON,O, and ABON,C(carbene) based on a rigid and tunable 2-arylbenzo[d]oxazole backbone have been prepared for the N-methylation of amines. Among these three coordinated modes, ABON,C(carbene)-chelated iridium-based catalysts exhibited good performance in the monomethylation of aromatic amines with methanol (MeOH) as the green methylation reagent. The steric-modified synthesis of ABON,C(carbene) complexes was described. The most active ABON,C(carbene) complex with marginal steric hindrance as a catalyst was obtained from the benzoxazole ring without a substituent and methyl group of the benzimidazole ring on the N-heterocyclic carbene (NHC) ligand. A variety of amines including para- and meta-substituted aromatic amines, as well as heterocyclic amines, were formulated as suitable substrates. Importantly, this catalyst considerably promoted the yield of the N-methylation of ortho-substituted aromatic amines. Controlled kinetic experiments and deuterium-labeling reactions of these ortho-substituted amines were conducted under optimized conditions. On the basis of the experimental results, a plausible mechanism was proposed.
- Huang, Shuang,Hong, Xi,Cui, He-Zhen,Zhou, Quan,Lin, Yue-Jian,Hou, Xiu-Feng
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p. 5072 - 5082
(2019/04/17)
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- Iron-Catalyzed Regioselective α-C-H Alkylation of N-Methylanilines: Cross-Dehydrogenative Coupling between Unactivated C(sp3)-H and C(sp3)-H Bonds via a Radical Process
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The iron-catalyzed α-C-H alkylation of N-methylanilines without any directing group by cross-dehydrogenative coupling between unactivated C(sp3)-H and C(sp3)-H bonds has been established for the first time, which provides a good complement to C(sp3)-H activation reactions and expands the field of Fe-catalyzed C-H functionalizations. Many different C(sp3)-H bonds in cyclic alkanes, cyclic ethers, and toluene derivatives can be used as coupling partners. Mechanistic investigations including the radical reaction process, the main role of various reagents, and the kinetic isotope effect experiment were also described.
- Li, Ze-Lin,Sun, Kang-Kang,Wu, Peng-Yu,Cai, Chun
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p. 6830 - 6839
(2019/06/14)
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- Manufacturing method for halogen substituted N-methylaniline
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The present invention relates to a method for manufacturing halogen-substituted N-methylaniline from halogen-substituted aniline. When halogen-substituted N-methylaniline is manufactured by using the method of the present invention, it is possible to manufacture halogen-substituted N-methylaniline without using existing methoxide sodium which has low chemical stability and is expensive, by using a low-cost base having excellent chemical stability such as potassium hydroxide or sodium hydroxide. Therefore, it is possible to reduce costs in a manufacturing process and to produce N-methylaniline with a high yield and high purity, thereby being useful for mass production as a raw material for herbicide metamifop synthesis.COPYRIGHT KIPO 2019
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Paragraph 0025-0030; 0043
(2019/09/05)
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- The design, synthesis and evaluation of selenium-containing 4-anilinoquinazoline hybrids as anticancer agents and a study of their mechanism
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Inhibition of tubulin polymerization is one of the significant strategies in the treatment of cancer. Inspired by the excellent antitumor activity of EP128495 and the beneficial biological activities of selenium compounds, a series of new selenium-containing 4-anilinoquinazoline hybrids were synthesized and evaluated as tubulin polymerization inhibitors. An anti-proliferative activity assay showed that most of the compounds inhibited human sensitive cancer cells at low nanomolar concentrations. A mechanism study revealed that the optimal compound 5a disrupted microtubule dynamics, decreased the mitochondrial membrane potential and arrested HeLa cells in the G2/M phase, finally resulting in cellular apoptosis.
- An, Baijiao,Zhang, Shun,Hu, Jinhui,Pan, Tingting,Huang, Ling,Tang, Johnny Cheuk-On,Li, Xingshu,Chan, Albert S. C.
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p. 4701 - 4714
(2018/07/03)
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- Formation of Phenyliodonio-Substituted Spirofurooxindole Trifluoroacetates from N-Substituted 3-Oxopentanediamides via Phenyliodine Bis(trifluoroacetate)-Mediated Oxidative Cascade Reactions
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The reaction of N-substituted 3-oxopentanediamides with phenyliodine bis(trifluoroacetate) (PIFA) was found to give a novel class of phenyliodonio-substituted spirofurooxindole trifluoroacetates under metal-free conditions. The reaction is postulated to proceed via a cascade process involving an oxidative C—O bond formation, an oxidative C—C bond formation and a final iodination step. (Figure presented.).
- Hu, Bei,Cao, Yang,Zhang, Bobo,Zhang-Negrerie, Daisy,Du, Yunfei
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supporting information
p. 2542 - 2548
(2017/08/16)
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- Stereospecific copper-catalyzed domino ring opening and sp3 C-H functionalization of activated aziridines with N-alkylanilines
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Copper efficiently catalyzed nucleophilic ring opening, sp3 C-H functionalization, and C-N bond formation in the presence of tert-butyl hydroperoxide to afford functionalized imidazolidines starting from N-sulfonylaziridines and Nalkylanilines. The products were obtained in high optical purities (95 → 99% ee) with excellent functional group tolerance.
- Sengoden, Mani,Bhowmick, Abhisikta,Punniyamurthy, Tharmalingam
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supporting information
p. 158 - 161
(2017/11/27)
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- Rhodium catalyzed regioselective arene homologation of aryl urea via double C–H bond activation and migratory insertion of alkyne
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A convenient rhodium catalyzed oxidative arene homologation of aniline derivatives with symmetrical or unsymmetrical alkynes using Cu(OAc)2as oxidant is described. Urea group is shown to be effective as a directing group for initial ortho C–H activation. Two migratory insertion events of alkyne into Rh–C bond occur successively, both with complete regioselectivity. This method is particularly useful for synthesis of polyarenes with different substituents, which has not been reported with conventional protocol. A mechanism has been proposed to explain the observed data.
- Wang, Yan,Zhou, Hao,Xu, Ke,Shen, Mei-Hua,Xu, Hua-Dong
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supporting information
p. 92 - 96
(2017/01/12)
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- Methylation of aniline and its derivatives with dimethyl carbonate in the presence of binder-free micro-, meso-, and macroporous zeolites KNaX, NaY, and HY
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Aniline and its derivatives undergo methylation when treated with dimethyl carbonate in the presence of binder-free micro-, meso-, and macroporous zeolites KNaX, NaY, and HY leading to the formation of N-methyl- and N,N-dimethylanilines.
- Khusnutdinov,Shchadneva,Mayakova, Yu. Yu.,Ardieva,Khazipova,Kutepov
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p. 1565 - 1570
(2017/01/28)
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- Room-temperature copper-catalyzed arylation of dimethylamine and methylamine in neat water
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The first room-temperature copper-catalyzed arylations of dimethylamine and methylamine in neat water have been developed. Using a combination of CuI and 6,7-dihydroquinolin-8(5 H)-one oxime as catalyst, dimethylamine is arylated with various aryl halides to give the corresponding products in good to excellent yields. Further, this catalysis enables the selective arylation of methylamine to afford the high yields of monoarylated methylamines as the sole products.
- Wang, Deping,Kuang, Daizhi,Zhang, Fuxing,Yang, Chunlin,Zhu, Xiaoming
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supporting information
p. 714 - 718
(2015/03/18)
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- Mn(III)-based oxidative cyclization of N-aryl-3-oxobutanamides. facile synthesis and transformation of substituted oxindoles
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The oxidation of 3-oxo-N-phenylbutanamides 1 with manganese(III) acetate in ethanol afforded dimeric 3,3'-biindoline-2,2'-dione derivatives 3-5. A similar reaction of N,2-disubstituted N-aryl-3-oxobutanamides 6 in acetic acid produced 3-acetylindolin-2-ones 7 bearing various substituents in good to excellent yields. The acetylindolinones 7 were easily deacetylated by treatment using neutral alumina in diethyl ether. Both the acetylindolinones 7 and deacetylated indolinones 8 were transformed by reduction into the substituted 1H-indoles.
- Kikue, Nobutaka,Takahashi, Tetsuya,Nishino, Hiroshi
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p. 540 - 562
(2015/03/04)
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- A High-Throughput Assay for Arylamine Halogenation Based on a Peroxidase-Mediated Quinone-Amine Coupling with Applications in the Screening of Enzymatic Halogenations
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Arylhalides are important building blocks in many fine chemicals, pharmaceuticals and agrochemicals, and there has been increasing interest in the development of more "green" halogenation methods based on enzyme catalysis. However, the screening and development of new enzymes for biohalogenation has been hampered by a lack of high-throughput screening methods. Described herein is the development of a colorimetric assay for detecting both chemical and enzymatic arylamine halogenation reactions in an aqueous environment. The assay is based on the unique UV/Vis spectrum created by the formation of an ortho-benzoquinone-amine adduct, which is produced by the peroxidase-catalysed benzoquinone generation, followed by Michael addition of either a halogenated or non-halogenated arylamine. This assay is sensitive, rapid and amenable to high-throughput screening platforms. We have also shown this assay to be easily coupled to a flavin-dependent halogenase, which currently lacks any convenient colorimetric assay, in a "one-pot" workflow.
- Hosford, Joseph,Shepherd, Sarah A.,Micklefield, Jason,Wong, Lu Shin
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supporting information
p. 16759 - 16763
(2016/02/12)
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- Selective methylation of amines with carbon dioxide and H2
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Put a label on it: Carbon dioxide with H2 is shown to be an efficient and selective methylation reagent for aromatic and aliphatic amines (see scheme; acac=acetylacetonate, triphos = 1,1,1- tris(diphenylphosphanylmethyl)ethane). A variety of functionalized amines including 13C-labelled drugs were obtained with good yields and functional-group tolerance. Copyright
- Li, Yuehui,Sorribes, Ivan,Yan, Tao,Junge, Kathrin,Beller, Matthias
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supporting information
p. 12156 - 12160
(2013/12/04)
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- One-pot synthesis of N,N-dimethylanilines from nitroarenes with skeletal Cu as chemoselective catalyst
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A range of N,N-dimethylanilines were synthesized with excellent yields in one-pot by the hydrogenation and alkylation of nitroarenes with H2 and HCHO over quenched skeletal Cu catalyst, which provides a facile, economical, and environmentally benign alternative methodology for C-N bonds formation.
- Rong, Zeming,Zhang, Wenjun,Zhang, Peng,Sun, Zhuohua,Lv, Jinkun,Du, Wenqiang,Wang, Yue
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p. 115 - 118
(2013/09/02)
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- Bicyclic core estrogens as full antagonists: Synthesis, biological evaluation and structure-activity relationships of estrogen receptor ligands based on bridged oxabicyclic core arylsulfonamides
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Compounds that block estrogen action through the estrogen receptor (ER) or downregulate ER levels are useful for the treatment of breast cancer and endocrine disorders. In our search for structurally novel estrogens having three-dimensional core scaffolds, we found some compounds with a 7-oxabicyclo[2.2.1]heptene core that bound well to the ERs. The best of these compounds, a phenyl sulfonate ester (termed OBHS for oxabicycloheptene sulfonate), was a partial antagonist on both ERα and ERβ. Although OBHS bears no structural resemblance to other estrogen antagonists, it appears to achieve its partial antagonist character by stabilizing a novel conformation of the ER that involves a significant distortion of helix-11. To enhance the antagonist properties of these oxabicyclo[2.2.1]heptane core ligands, we expanded the functional diversity of OBHS by replacing the sulfonate with secondary or tertiary sulfonamides (-SO2NR-), isoelectronic and potentially isostructural molecular replacements. An array of 16 OBHS sulfonamide analogues were prepared through a Diels-Alder reaction of a 3,4-diarylfuran using various N-aryl vinyl sulfonamide dienophiles. While the more polar secondary sulphonamides were weak ligands, certain of the tertiary sulfonamides had very good ER binding affinity. In HepG2 cell reporter gene assays, the sulphonamides had moderate potency, but they showed lower intrinsic transcriptional activity on ERα than the selective estrogen receptor modulator (SERM) hydroxytamoxifen or OBHS, and they were inverse agonists on ERβ. Thus, the behaviour of these OBH-sulfonamides more closely mirrors the activity of full antagonists like the drug fulvestrant (ICI 182780), and their greater antagonist biocharacter appears to arise from an accentuated distortion of helix-11.
- Zhu, Manghong,Zhang, Chen,Nwachukwu, Jerome C.,Srinivasan, Sathish,Cavett, Valerie,Zheng, Yangfan,Carlson, Kathryn E.,Dong, Chune,Katzenellenbogen, John A.,Nettles, Kendall W.,Zhou, Hai-Bing
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supporting information
p. 8692 - 8700
(2013/01/15)
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- A facile and practical copper powder-catalyzed, organic solvent-and ligand-free ullmann amination of aryl halides
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A facile and practical method that the copper powder-catalyzed Ullmann amination of aryl halides with aqueous methylamine under organic solvent-and ligand-free condition at 100 °C and in air gave N-arylamines as sole products in good to excellent yields. The presence of a small amount of air is essential. Other aliphatic primary amines show good to very high reactivity. Secondary amines and aniline are not reactive. Sensitive substituents (i.e., CHO, MeCO, CN and Cl) are tolerable in the reaction.
- Jiao, Jiao,Zhang, Xi-Ru,Chang, Ning-Hui,Wang, Jie,Wei, Jun-Fa,Shi, Xian-Ying,Chen, Zhan-Guo
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supporting information; experimental part
p. 1180 - 1183
(2011/04/24)
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- A facile protocol for the synthesis of mono-N-methyl anilines via formimidate intermediates
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A general procedure for the preparation of mono-N-methyl anilines has been developed with excellent yields. This protocol relies on a NaBH3(OAc) reduction of formimidate intermediates that are quantitatively generated by treatment of primary substituted anilines with triethyl orthoformate under the catalysis of MCM-41-SO3H mesoporous zeolite. The newly developed procedure was facile, efficient, and environmentally benign.
- Sun, Nan,Wang, Shuai,Mo, Weimin,Hu, Baoxiang,Shen, Zhenlu,Hu, Xinquan
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experimental part
p. 7142 - 7148
(2010/09/14)
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- Metal organic frameworks as heterogeneous catalysts for the selective N-methylation of aromatic primary amines with dimethyl carbonate
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Metal organic frameworks (MOFs) with aluminium, copper and iron as central metal atoms with 1,4-benzenedicarboxylic acid (aluminium) and 1,3,5-benzenetricarboxylic acid (copper and iron) as ligands are selective and active catalysts in promoting the polymethylation of aromatic amines with dimethyl carbonate (DMC). N-methylation prevails over carbamoylation even though they are competing parallel processes. The present N-methylation protocol using DMC enjoys advantages such as convenient reaction conditions, benign, reusable, cost-effective catalyst, avoids the use of additional solvent and uses a safe, green methylating agent that only produces CO2 and methanol as by-products.
- Dhakshinamoorthy, Amarajothi,Alvaro, Mercedes,Garcia, Hermenegildo
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experimental part
p. 19 - 25
(2010/08/20)
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- IBiox[(-)-menthyl]: A sterically demanding chiral NHC ligand
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(Figure Presented) An exceedingly sterically demanding, rigid, and chiral NHC ligand, IBiox[(-)-menthyl] (1), was prepared and structurally characterized. With a buried volume of 50percent, this ligand arguably represents one of the most sterically demanding monodentate ligands. The ability to use aryl chloride substrates in intramolecular palladium-catalyzed ,-arylations reveals its unique reactivity. Moreover, C2-symmetric 1 allows the highly enantioselective formation of oxindoles withup to 99percent ee.
- Wuertz, Sebastian,Lohre, Claudia,Froehlich, Roland,Bergander, Klaus,Glorius, Frank
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supporting information; experimental part
p. 8344 - 8345
(2009/10/24)
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- THIADIAZOLE DERIVATIVES, INHIBITORS OF STEAROYL-COA DESATURASE
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The present invention relates to substituted thiadiazole compounds of the formula (I) and pharmaceutically acceptable salts thereof, to pharmaceutical compositions containing them and their use in medicine. In particular, the invention relates to compounds for modulating SCD activity.
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Page/Page column 90-91
(2008/12/07)
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- Synthesis of functionalized indole- and benzo-fused heterocyclic derivatives through anionic benzyne cyclization
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The development of a new method for the regioselective synthesis of functionalized indoles and six-membered benzo-fused N-, O-, and S-heterocycles is reported. The key step involves the generation of a benzyne-tethered vinyl or aryllithium compound that undergoes a subsequent intramolecular anionic cyclization. Reaction of the organolithium intermediates with selected electrophiles allows the preparation of a wide variety of indole, tetrahydrocarbazole, dihydrofenantridine, dibenzopyran, and dibenzothiopyran derivatives. Finally, the application of this strategy to the appropriate starting materials allows the preparation of some tryptamine and serotonin analogues.
- Barluenga, Jose,Fananas, Francisco J.,Sanz, Roberto,Fernandez, Yolanda
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p. 2034 - 2046
(2007/10/03)
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- Synthesis of 4-functionalized indoles via benzyne cyclization of N-(2- lithioallyl)-2-fluoroanilines
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Treatment of N-(2-bromoallyl)-N-methyl-2-fluoroaniline with tert- butyllithium affords 1,3-dimethyl-4-lithioindole, via intramolecular addition to a tethered benzyne intermediate. Further reaction with electrophiles leads to 4-functionalized 3-methylindol
- Barluenga, Jose,Fananas, Francisco J.,Sanz, Roberto,Fernandez, Yolanda
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p. 1049 - 1052
(2007/10/03)
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- t-butyl hypochlorite: A powerful electrophilic aromatic ring chlorinating agent
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t-Butyl hypochlorite is an excellent aromatic ring chlorinating agent, under mild conditions, without any catalyst, of acetanilide. High regioselectivity is observed, the product being, nearly exclusively, para- chloroacetanilide.
- Lengyel, Istvan,Cesare, Victor,Stephani, Ralph
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p. 1891 - 1896
(2007/10/03)
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- N-methyl-N-phenylnitrenium ion from photolysis of N-(methylphenylamino)-2,4,6-trimethylpyridinium tetrafluoroborate
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The photochemical reactions of N-(methylphenylamino)-2,4,6-trimethylpyridinium tetrafluoroborate were studied to find evidence of photodecomposition to a nitrenium ion reactive intermediate. Stable products were formed that were consistent with a singlet-state methylphenylnitrenium ion precursor. The methoxy and chloro adducts. N-methyl-p-anisidine and 4- (and 2-)chloro-N-methylaniline, were identified and quantified by high-performance liquid Chromatographic analysis. A hydride shift from the N-methyl group of the nitrenium ion is also proposed based on the detection of aniline which would result from hydrolysis of the iminium ion rearrangement product. The rate constant for this rearrangement is estimated to be 108s-1. The reduction product, N-methylaniline, is produced, and is believed to form, at least in part, from the hydrogen atom abstractions of the triplet nitrenium ion. This is supported by the results of triplet sensitized irradiations. Laser flash photolysis studies yielded the transient spectrum of a long-lived intermediate absorbing at 470 nm. This transient species is believed to be the cation radical of N-methylaniline.
- Chiapperino,Falvey
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p. 917 - 924
(2007/10/03)
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- Preparation of Hybrid Bidentate Phosphine Ligands by Reduction of Their Benzyl- or Phenyl-phosphonium Salts. X-Ray Crystal Structure of 2-Aminophenyltriphenylphosphonium Tetrachloronickelate(II)
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The 2-substituted phenylphosphine bidentate hybrid ligands, 2-aminophenyl-, 2-methylaminophenyl-, 2-hydroxyphenyl- and (2-amino-3-methylphenyl)-diphenylphosphine, (1a-d), respectively, and 2-aminophenylmethylphenylphosphine, (1e), were synthesized by reduction of their phenylphosphonium halides, (2a-e)X (X = Cl or Br), with sodium naphthalenide in tetrahydrofuran at -68 deg, or electrochemically at a mercury cathode.The phosphonium salts were prepared by reaction of triphenylphosphine with aryl halide and anhydrous nickel halide at 200 deg.X-Ray diffraction of (2a)2 showed it to have monoclinic space group P21/n, a 10.657(4), b 20.966(3), c 20.422(6) Angstroem, β 101.33(2) deg and Z 4.The structure was refined by a full-matrix least-squares procedure to a final R 0.050 for 3534 reflections with I > 2.5?(I).
- Cooper, Mervyn K.,Downes, J. Michael,Duckworth, Paul A.,Tiekink, Edward R. T.
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p. 595 - 609
(2007/10/02)
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