FeCl_3催化吲哚烯丙醇Nazarov环化合成新型稠环吲哚

以吲哚-2-甲醛和取代苯乙酮为原料,经3步反应合成了10个吲哚烯丙基醇(5a~5j);以Fe Cl3·6H2O为催化剂,二氯甲烷为溶剂,5于40℃经分子内Nazarov环化反应,合成了10个新型稠环吲哚(6a~6j),其结构经1H NMR,13C NMR和HR-ESI-MS表征。     

Fe(Ⅲ)催化的烯丙醇的Friedel-Crafts环化反应合成多取代茚

在FeCl3·6H2O催化下,多取代的烯丙醇可以顺利进行分子内Friedel-Crafts环化反应,以中等到优良的产率得到一系列多取代茚化合物,该反应操作简单、反应条件温和.产物结构经IR,1H NMR,13C NMR,HR MS及X射线单晶衍射分析确证.     

烯丙基转移反应合成直链高烯丙基醇

研究了不同脂肪族和芳香族醛与6-甲基-6-苯基-7-烯-1,5-辛二醇的烯丙基转移反应, 同时考察了溶剂对反应的影响. 结果发现, 在In(OTf)3催化下, 以甲苯为溶剂, 由脂肪族醛合成的直链高烯丙基醇较芳香族醛具有较高的产率和较好的选择性, 所得产物结构经1H NMR, 13C NMR, IR, HRMS表征.     

Palladium‐Catalyzed Allylic Alkylation of Simple Ketones with Allylic Alcohols and Its Mechanistic Study

Allylic alcohols were directly used in Pd‐catalyzed allylic alkylations of simple ketones under mild reaction conditions. The reaction proceeded smoothly at 20 °C by the concerted action of a Pd catalyst, a pyrrolidine co‐catalyst, and a hydrogen‐bonding solvent, and does not require any additional reagents. A computational study suggested that methanol plays a crucial role in the formation of the π‐allylpalladium complex by lowering the activation barrier.     

An Efficient Solvent-free Synthetic Technique of 4,4’-Diaminotriarylmethane Leuco Materials

An efficient, versatile and solvent-free synthetic technique of diaminotriarylmethanes was reached by treating N,N-dimethylaniline with some arylaldehydes over zirconium(IV) oxide chloride (ZrOCl2•8H2O), in which ZrOCl2•8H2O has good activity, easy availability, recovery as well as reusability.     

Study on the Phase Diagram of CsCl-CeCl3-HCl(11%)-H2O System and the Properties of the Compounds

The equilibrium solubility of CsCl-CeCl3-HCl(11%)-H2O qua-ternary system at 25℃ has been determined by the physicchemical analysis method ,and the phase diagram was plotted, Two new double salts 3CsCl.CeCl3.3H2O and CsCl.CeCl3.4H2O obtained from the complicated system were identified and characterized by XRD,TG-DTA ,DSC,UV and fluorescence spectroscopy, Studies on the fluorescence excitation and emission show that 3CsCl.CeCl3.3H2O and CsCl.CeCl3.4H2O have upconversion luminescence of infrared-visible range,and the upconversion emission intensity increases with the increase of ratio of CeCl3 in CsCl.     

Synthesis and Thermodynamic Properties of MgO·B_2O_3·4H_2O

ＩｎｔｒｏｄｕｃｔｉｏｎＴｈｅｒｅａｒｅｍａｎｙｋｉｎｄｓｏｆｍａｇｎｅｓｉｕｍｂｏｒａｔｅｓ ,ｂｏｔｈｎａｔｕｒａｌａｎｄｓｙｎｔｈｅｔｉｃ .Ａｂｏｒａｔｅｄｏｕｂｌｅｓａｌｔ (2ＭｇＯ·2Ｂ2 Ｏ3 ·ＭｇＣｌ2 · 14Ｈ2 Ｏ)ｎａｍｅｄｃｈｌｏｒｏｐｉｎｎｏｉｔｅｗａｓｏｂ ｔａｉｎｅｄｆｒｏｍｔｈｅｎａｔｕｒａｌｃｏｎｃｅｎｔｒａｔｅｄｓａｌｔｌａｋｅｂｒｉｎｅ .1Ｉｎｏｒｄｅｒｔｏｆｉｎｄｔｈｅｆｏｒｍｉｎｇｒｅｌａｔｉｏｎｂｅｔｗｅｅｎｔｈｅｄｏｕｂｌｅｓａｌｔａｎｄｍａｇｎｅｓｉｕｍ ｂｏｒａ…     

合成烯丙基芳基硒醚的一种简便方法——烯丙基锌与二芳基二硒醚反应

烯丙基溴与锌粉在0～10 ℃下THF中反应生成烯丙基锌，后者与二芳基二硒醚 在THF中、室温下反应生成烯丙基芳基硒醚，产率63%～75%。     

FeCl_3催化合成新型烯丙基醚类化合物

以烯丙基醇类化合物(1a~1i)和乙醇为起始原料,FeCl_3为催化剂,经分子间亲核取代反应合成了9个烯丙基醚类化合物(2a~2i,其中2c,2e~2i为新化合物),收率80%~95%,其结构经1H NMR,13C NMR和HRESI-MS表征。研究了催化剂,溶剂,反应温度和反应时间对2a产率的影响。结果表明:在最优反应条件[1a 0.5mmol,Fe Cl34 mg,Et OH 2.5 mmol,CH2Cl2为溶剂,于室温反应0.8 h]下,2a收率95%。     

Chiral Primary Amine/Palladium Dual Catalysis for Asymmetric Allylic Alkylation of β‐Ketocarbonyl Compounds with Allylic Alcohols

An efficient dual catalytic system composed of a chiral primary amine and a palladium complex was developed to promote the direct asymmetric allylic alkylation (AAA) of β‐ketocarbonyl compounds. In particular, the synergistic dual catalytic system enabled the AAA reaction of challenging acyclic aliphatic ketones, such as β‐ketocarbonyl compounds and 1,3‐diketones.     

One-Pot Synthesis of 2,3-Diarylbenzofurans via Sequential Iodocyclization and Pd-Catalyzed Suzuki Coupling Reactions of 2-Alkynylanisoles with Boronic Acids in Water

An efficient approach for the one-pot synthesis of 2,3-diarylbenzofurans via sequential iodocyclization and Pd-catalyzed Suzuki coupling reaction of 2-alkynylanisoles with boronic acids in water is reported. The protocol utilizes water as the solvent and there is no need to isolate the intermediate 3-iodine-2-arylbenzofurans, which exemplifies the ideal of green chemistry. Various 2-alkynylanisoles and boronic acids can participate in the reactions, providing a series of 2,3-diarylbenzofurans for drug discovery in moderate to good yields.     

A Sustainable Synthesis of 2‐Benzoxazyl and 2‐Benzothiazyl Ketones from Alkynyl Bromides and 2‐Amino(thio)phenols Promoted by a Recyclable Catalytic System

An environmentally and economically sustainable synthesis of 2‐benzoxazyl ketones and 2‐benzothiazyl ketones through FeCl₃·6H₂O catalyzed tandem reactions of alkynyl bromides with 2‐amino(thio)phenols in [bmim]BF₄ has been developed. Remarkable advantages of this new synthetic strategy include high efficiency, readily available starting materials, and recyclable catalyst and reaction medium.     

Arylation of Allylic Alcohols with Aryl Iodides Catalyzed by a Silica-Bound Bidentate Sulfur Palladium (0) Complex

Thepalladium-catalyzedarylation0fallylicalc0h0lswitharylhalideshaspr0videdaconvenientmethodforthesynthesisof3-arylaldehydesandket0nesl'2.Benhaddouetal.3havestudiedthekineticsofthisarylationreaction.H0wever,homogene0uspalladiumcatalystssuchasPd(0Ac)2andPdCl2areusuallyused,anditisdifficulttorecuverthemfromthereactionmixture.ThemethodofinunobilizingcomPlexeshasmadehomogeneouscatalystsgenerallymoreattractivefromtheoreticalandindustrialpointsofview.Polymer-supportedpalladiumcatalystshavebeensucce…     

Synthesis and crystal structure of a complex bearing interesting structural motifs: [Cu (C4H7N3) H2O (4,4′-Hbpy)]·SO4·NO3

A new complex [Cu (C₄H₇N₃) H₂O (4,4′-Hbpy)]·SO₄·NO₃ was synthesized and X-ray characterized. Elemental analysis, X-ray diffraction and infrared spectroscopy of the complex were performed. The crystal system is orthorhombic. Crystal data: Fw=498.98, spacegroup: P212121. Z=4, a=14.952(3), b=20.491(4), c=6.713 Å. V=2056.7(9) Å. λ(Mo-K)=0.71070 Å. μ=12.18 cm⁻¹, D_calc=1.66 g/cm³, F₀₀₀=1032.00, R=0.062, Rw=0.087. X-ray analysis illustrated that 4,4′-bpy is mono-protonated and that there are two kinds of anions in one molecule, which give rise to the hydrogen interaction between the molecules in the crystal. Then an extended three-dimensional network is formed along the hydrogen bonds and π–π bonds between the pyridine rings.     

铜催化肟酯与苄醇构建多取代吡啶

以肟酯和苄醇为反应物,三氟甲磺酸铜[Cu(OTf)₂]为催化剂,通过“一锅法”反应合成三取代吡啶化合物。 分别考察了不同催化剂及其用量、原料配比、溶剂及温度对反应的影响,在最优条件下,反应的收率为85%,目标化合物经核磁共振氢谱、核磁共振碳谱以及质谱进行了结构表征。 该方法具有原料易得,操作简单,反应条件简单温和,产物收率高以及底物适用性好等优点。     

CuCl‐Catalyzed Aerobic Oxidation of Allylic and Propargylic Alcohols to Aldehydes or Ketones with 1:1 Combination of Phenanthroline and Bipyridine as the Ligands

We developed a modified protocol for the oxidation of 2,3‐allenyl alcohols using CuCl with 1:1 combination of phenanthroline and bipyridine as the catalyst. To further investigate the applicability of this system, other types of alcohols such as allylic and propargylic alcohols have been tested: we found that both allylic and propargylic alcohols may be oxidized to the corresponding aldehydes or ketones using molecular oxygen in air as the oxidant with moderate to excellent yields.     

新型香豆素类荧光化合物的合成及荧光性质研究

合成了两种香豆素类荧光化合物6,8-二氯-7-羟基香豆素-3-羧酸（DClC）和6-氯-7-羟基香豆素-3-羧酸（MClC）,其中DClC未见文献报道,并通过红外光谱、核磁共振、质谱等手段对产物的结构进行了表征。同时首次研究了这两种香豆素衍生物的紫外、荧光性质,以及不同极性溶剂、pH值、表面活性剂等的影响。结果表明,pH对性质测定影响较大,当pH=10时,DClC和MClC的荧光强度明显增强。     

Synthesis of 11H-Indeno[1,2-b]quinolines via the Friedliinder Reaction

The nine new 11H-indeno[1,2-b]quinolines were synthesized in high yield with sodium ethoxide as a catalyst via the Friedlander condensation reaction, The possible reaction mechanism was proposed.