Pd-catalyzed sequential reaction for the synthesis of fused tricyclic compounds containing a dihydrofuran or isobenzofuranone unit

A novel Pd-catalyzed sequential reaction for the synthesis of fused tricyclic compounds with a dihydrofuran or isobenzofuranone unit was developed.

Addition of Allyltrimethylsilane to tert-Butanesulfinyl Imines Triggered by Tetra-n-butylammonium Fluoride

The addition of allyltrimethylsilane to tert-butanesulfinyl imines triggered by tetra-n-butylammonium fluoride （TBAF） in the presence of 4A molecular sieves has been studied, and homoallylsulfinamides were obtained in good yields with moderate to high diastereoselectivities.

Facile and Stereoselective Synthesis of N-Substituted Benzotriazole with Baylis-Hillman Adducts

A convenient method has been developed toward the stereoselective synthesis of N-substituted benzotriazole derivatives under mild conditions. The good stereolectivity, high yields and the simple procedure make the present protocol attractive.

The Reductive Addition Reaction of Substituted 2-Chloromethyl-1,3,4-oxadiazole to Aldehydes and Ketones Promoted by Samarium Diiodide

1-（β-Hydroxyalkyl）-l,3,4-oxadiazole derivatives were synthesized via reductive addition reactions of 2-chloromethyl-l,3,4-oxadiazole with carbonyl compounds under mild conditions promoted by SmI2.

Study on the reactions of azo compounds with acyl halides mediated by Sm/TiCl_4

Amides can be obtained in good to excellent yield by Sm/TiCl4 mediated reductive cleavage of N=N bond in azo compounds and successive acylation in one pot. It offers an alternative method for the synthesis of amides from very simple starting materials directly.

Studies on K2CO3-Catalyzed 1,4-Addition of 1,2-Allenic Ketones with Diethyl Malonate: Controlled Selective Synthesis of β, γ-Unsaturated Enones and α-Pyrones

The reaction of diethyl malonate with various substituted 1,2-allenic ketone can be catalyzed by 10% of K2CO3leading to polyfunctionalized β, γ-unsaturated enones 3 or 4. With 3-unsaturated 1-substituted-1, 2-allenic ketones, the highly selective formation of β, γ-unsaturated enones 4 was observed; with 1,2-allenic ketones with one or two γ-substituents, only β, γ-unsaturated enones 3 with an unmigrated carbon-carbon double bond were produced; with γ-monosubstituted-1,2-allenic ketones the corresponding (E)-3 were formed highly selectively; with propadienyl ketones, a mixture of β, γ-unsaturated enones 3 and 4 were formed.……

Regio- and stereo-selective synthesis of multi-substituted 3-pyrrolines

A regio- and stereo-selective synthesis of multi-substituted 3-pyrrolines has been developed. The multi-substituted 3-pyrrolines were synthesized in good yields by 1,3-dipolar cycloaddition of methyl 2-（phenylselanyl）acrylate with azomethine ylides, followed by N-acylation and oxidation-elimination of phenylseleno group. 2009 Xian Huang. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

The facile insertion of β-keto sulfones to arynes:The direct preparation of polysubstituted ortho-keto benzyl sulfones

One novel carbon-carbon bond insertion reaction of arynes has been developed. By this reaction β-keto sulfones can insert the triple bond of arynes to prepare polysubstituted ortho-keto benzyl sulfones.

Synthesis and Crystal Structure of an Incomplete Cubane-like Heterobimetallic Cluster [（η^5-C5Me5）2Mo2（μ3-S）（μ-S）3（CuCl）]

The reaction of[（η^5-C5Me5）2Mo2（μ3-S）（μ-S）3（CuCl）]1 with Na2S in MeCN produced a trinuclear cluster [（η^5-C5Me5）2Mo2（μ3-S）（μ-S）3（CuCl）] 2. 2 crystallizes in the monoclinic system, space group P21/c with a = 15.563（3）, b = 8.9547（18）, c = 17.846（4） A, β = 101.29（3）°, V = 2438.9（9） A^3, Z = 4, Dc = 1.878 g/cm^3, T = 193（2） K, C20H30ClCuMo2S4, Mr = 689.60, F（000） = 1376, μ（MoKa） = 2.335 mm ^-1, S = 1.050, R = 0.0305 and wR = 0.0688 for 4033 observed reflections with I 〉 20-（I）. In the structure of 2, one [（η^5-C5Me5）2Mo2（μ-S）2S] moiety and one CuCI unit are assembled into an incomplete cubane-like [Mo2S4Cu] core framework, in which the Cu center adopts a distorted tetrahedral geometry coordinated by one ,μ3-S atom, two μ-S atoms and one terminal chloride. The two Mo…Cu contacts are 2.7519（7） and 2.7689（8） A, respectively.

Selective Deoxygenation of Nitrones Mediated by Sm/CoCl_26H_2O Reductive System

In the presence of metallic samariumcobalt (II) chloride hexahydrate, the nitrones can be reduced to the corresponding imines in moderate to high yields under mild and neutral conditions.

Crystal Structure of (E,E)-1,10-Bis-(4-fluoro-phenyl)-3,8-dimethyl-deca-3,7-diene-1,10-dione

The crystal and molecular structures of (E,E)-1,10-bis-(4-fluorophenyl)-3,8-dime- thyl-deca-3,7-diene-1,10-dione have been determined by X-ray diffraction method. The crystal (C24- H24F2O2, Mr = 382.45) is of monoclinic, space group P21/c, a = 11.0392(5), b = 11.3620(4), c = 7.9361(3) ?, β = 97.423(2)o, V = 987.06(7) ?3, Z = 2, Dc = 1.287 g/cm3, μ(Mo-Kα) = 0.93 cm-1, λ = 0.7107 ?, F(000) = 404.00, the final R = 0.0530 and wR = 0.150 for 1348 observed reflections (I > 2σ(I)). X-ray analysis revealed that there exists a double bond in C(9)–C(11) with the bond length of 1.324(3) ?, while the C(8)–C(9) bond length is 1.508(3) ? and it may be assigned to a single bond. These results show that the C=C bond is not conjugated with the C=O bond.

Synthesis and Crystal Structure of {η~5:η~1-[(2-Methoxyphenyl)-isopropyl]-indenyl}(dimethoxyethylene)lithium1

The title compound {η^5：η^1-[（2-MeOC6H4）C3H6]CgH6}Li（DME） （DME=1,2-dimethoxy-ethylene） was synthesized by the treatment of 3-[（2-methoxyphenyl）-isopropyl]-indene with 1 equiv, of n-BuLi followed by the recrystallization from a mixed solution of toluene and DME. The compound crystallizes in orthorhombic system, pace group Pbca with a=14.5677（3）, b=15.54670（10）, c=18.7498（3）A°, Z=8, V=4246.45（11）A°^3, Dc=1.127 g/cm^3 and μ（MoKα）=0.072 mm^-1. The coordination geometry can be described as a distorted tetrahedron.

An Efficient Synthesis of 4-Halo-5-hydroxyfuran-2(5H)-ones via the Sequential Halolactonization and γ-Hydroxylation of 4-Aryl-2,3-alkadienoic Acids

5-Hydroxyfuran-2(5H)ones are an important class of compounds because they often occur in natural products and exhibit a broad range of biological activities. Recently, much attention has been focused on the efficient and di verse synthesis of these compounds, particularly 4-halo-5-hydroxy-2(5H)-furanones. The typical synthetic strategies include acid catalyzed cyclization of ketonic acids, auto oxidation of corresponding lactone in air, rearrangement reactions of α-phenylsulphinylacrylates, oxidation with chromium trioxide in acetic acid, and bromination-hydrolysis of α ,β-butanolides. Herein, we wish to report that 4-halo-5-hydroxyfuran-2(5H)-ones were synthesized via the efficient sequential halolactonization-hydroxylation reaction of 4-aryl-2,3-allenoic acids with I2 or CuX2 (X = Br or Cl) inmoderate to good yields.……

A General and Efficient Enantioselective Total Synthesis of Four Stereoisomers of Lupinine

Bicyclic alkaloids having izidine skeletons, are widely observed in various plant families, which show tumor inhibitory activity.……

Efficient Synthesis of Bi-butenolides Derivatives through Oxidative Dimeric Cyclizing-Coupling Reaction of 2,3-Allenoic Acids

Allenes are three carbon functional groups possessing two perpendicular π-orbitals. Their unique reaction be havior is spread over three carbon atoms, which shows great potential in organic synthesis in terms of chirality transfer and diversity, as a result of the axial chirality as well as the substituent-loading capability. Recently, we devoted ourselves to establish a new area of oxidative cyclization-dimerization reactions between two functionalized allenes to give interesting bicyclic compounds in a single step. The formidable challenges are to match the reactivities of two allenes, and regenerate the catalyst, which would be reduced after reductive-elimination. In this paper we wish to disclose our recent studies on the synthesis of bi-butenolides from oxidative cyclization self-coupling reaction of 2,3 allenoic acids, in which a new system (PdCl2/RI/air) for regeneration of the palladium(Ⅱ) species was observed.……

First Palladium-Catalyzed Addition of Organoboronic Acids to Allenes: A Magic Regioselectivity Switch by Using a Base or an Acid

Organoboronic acids enjoy high prestige in the metal-catalyzed C-C bond formations. The most notable progress is the rhodium- and nickel-catalyzed conjugate addition with unsaturated carbon-carbon bond, aldehydes, N-sulfonyl imines reported by Miyaura, Hayashi and Shirakawa.[1]……

Ultralong nitrogen/sulfur Co-doped carbon nano-hollowsphere chains with encapsulated cobalt nanoparticles for highly efficient oxygen electrocatalysis

The development of simple and effective strategies to prepare electrocatalysts,which possess unique and stable structures comprised of metal/nonmetallic atoms for oxygen reduction reaction(ORR)and oxygen evolution reaction(OER),is currently an urgent issue.Herein,an efficient bifunctional electrocatalyst featured by ultralong N,S-doped carbon nano-hollow-sphere chains about 1300 nm with encapsulated Co nanoparticles(Co-CNHSCs)is developed.The multifunctional catalytic properties of Co together with the heteroatom-induced charge redistribution(i.e.,modulating the electronic structure of the active site)result in superior catalytic activities toward OER and ORR in alkaline media.The optimized catalyst Co-CNHSC-3 displays an outstanding electrocatalytic ability for ORR and OER,a high specific capacity of 1023.6 mAh gZn^(-1),and excellent reversibility after 80 h at 10mA cm^(-2)in a Zn-air battery system.This work presents a new strategy for the design and synthesis of efficient multifunctional carbon-based catalysts for energy storage and conversion devices.