双消除法一锅简便合成1－丙炔基芳香化合物

报道了一种便捷合成1-丙炔基芳香化合物的新方法. 在充分探讨反应条件的基础上, 利用硫试剂乙基苯基砜与芳香醛组合, 采用双消除反应成功地一锅合成了一系列1-丙炔基芳香化合物1a～1s. 运用此法不仅合成出一些含有醚键、萘环、杂环以及含有两个1-丙炔基的化合物, 重要的是芳环上含有卤原子(Br和I)的化合物也能顺利地合成出来. 该方法原料易得, 操作简单, 产物容易分离纯化并且产率理想.     

由邻硝基苯胺一锅法合成苯并咪唑化合物

以邻硝基苯胺为原料, 在SnCl2•2H2O/KI/HCl体系中, 100 ℃条件下, 一锅法合成12种苯并咪唑化合物. 该方法以水为溶剂, 条件温和, 操作简单, 催化剂易得, 产率较高, 为该类化合物的合成提供了一种新的便利方法.     

Convenient, Efficient One-Pot Synthesis of Ferrocenylcyanide

In asymmetric catalysis, chiral (central chiral, planar chiral, axial chiral) ferrocenylligands is one of the most successful class of auxiliaries in recent years, and some ofthem have reached the stage of industrial applications'. But many challenges remain forthe synthesis of the intermediate. One of them is how to get ferrocenylcyanide I directlyfrom ferrocenecarboxyaldehyde 2, which can be easily prepared according to thecorresponding literature2. As far as known, I is an important interm…     

A Convenient One-Pot Synthesis of Di-t-butylphosphinic Chloride

A convenient one-pot synthesis of (t-Bu)₂P(O)Cl (1) from m-chloroperbenzoic acid and (t-Bu)₂PCl is described. The byproduct m-chlorobenzoic acid is neutralized by addition of Et₃N. Complex 1 crystallizes in the monoclinic space group P2₁/c (No. 14), with a = 5.9637(2) Å, b = 11.4734(4) Å, c = 16.2400(5) Å and β = 107.7160(14).     

一锅法合成4-(5-芳基-1,3,4-噻二唑-2-氨甲基)苯酚衍生物

以2-氨基-5-芳基噻二唑衍生物和对羟基苯甲醛为原料,经亲核加成/脱水、还原两步一锅法合成了一系列新的4-(5-芳基-1,3,4-噻二唑-2-氨甲基)苯酚衍生物,反应具有时间短、后处理简单等优点.采用元素分析,NMR,IR以及质谱等多种谱学技术对产物进行了详细表征.     

Novel One-Pot Synthesis of Functionalized (Z)-2-Arylvinyl Bromides

A novel and versatile one-pot synthesis of functionalized (Z)-2-arylvinyl bromides was developed. The new procedure involved microwave-induced debrominative decarboxylation of cinnamic acid dibromide with Et₃N and subsequent esterification in the presence of dicyclohexyl carbodiimide (DCC) and dimethyl-aminopyridine (DMAP).     

Simply Structured Near-Infrared Emitters with a Multicyano Linear Acceptor for Solution-Processed Organic Light-Emitting Diodes

Near-infrared (NIR) organic light-emitting diodes (OLEDs) show great potential in a variety of applications including sensors, night vision, and information security. Despite the superiority of thermally activated delayed fluorescence (TADF) in 100 % exciton harvesting, the development of NIR TADF OLEDs is still a great challenge, especially in terms of solution-processing technology. In this work, a multicyano acceptor of 2-dicyanomethylene-3-cyano-4,5,5-trimethyl-2,5-dihydrofurance (TCF) with strong electron-withdrawing ability was employed to construct solution-processible NIR emitters, CzTCF and tBCzTCF, with the feature of donor–π–acceptor (D –π–A) structure. The significantly enhanced intermolecular charge transfer effects not only render the deep-red and NIR emissions of CzTCF and tBCzTCF films, respectively, but also lead to their typical TADF characteristics. Consequently, the nondoped solution-processed NIR OLED based on tBCzTCF was successfully demonstrated with the peak wavelength of 715 nm, which paves the way for developing NIR emitters without polycyclic aromatic cores and heavy-metal ions.     

Sequence-Controlled Catalytic One-Pot Synthesis of Siloxane Oligomers

Silicones are highly valuable poly- and oligomeric materials with a broad range of applications due to their outstanding physicochemical properties. The core framework of silicone materials consists of siloxane (Si−O−Si) bonds, and thus, the development of efficient siloxane-bond-forming reactions has attracted much attention. However, these reactions, especially “catalytic” siloxane-bond-forming reactions that enable the selective formation of unsymmetrical siloxane bonds, remain relatively underdeveloped. On the other hand, controlled iteration has become a powerful tool for the sequence-controlled synthesis of poly- and oligomeric compounds. Recently, control over the siloxane sequence has been achieved by the one-pot iteration of a B(C₆F₅)₃-catalyzed dehydrocarbonative cross-coupling of alkoxysilanes with hydrosilanes and a B(C₆F₅)₃-catalyzed hydrosilylation of carbonyl compounds. Thus, it is now possible to generate linear, branched, and cyclic sequence-specific oligosiloxanes in a highly selective manner under chloride-free conditions.     

Efficient and Convenient One-Pot Synthesis of Dioxadiazaphophepines

The reaction of vicinal dioxime with sodium hydride in dry THF followed by addition of dichlorophosphates or dichlorothiophosphates yields 2-oxo-1,3,4,7-dioxadiazaphosphepines and 2-thioxo-1,3,4,7-dioxodiazaphosphepines in moderate to good overall yields. The products are characterized by elemental analyses, molecular weights and spectral (IR, ¹H, ¹³C and ³¹P NMR) studies. A salt elimination route is used for the synthesis of titled heterocycles.     

基于双“click”反应的树枝状化合物的一锅法合成

将叠氮和炔基之间Cu(I)催化的“click”反应以及蒽和马来酰亚胺之间的Diels-Alder反应相结合, 采用“一锅法”技术合成出结构完美且外围含有亲水性寡聚乙二醇(OEG)链段的树枝状化合物4, 产率为75%. 利用核磁共振氢谱、碳谱、紫外、荧光光谱以及MALDI-TOF质谱等对产物进行了表征与分析, 并利用凝胶渗透色谱(GPC)对其纯度进行了测试.     

Novel Dual Use of Formamide-POCl3 Mixture for the Efficient,One-Pot Synthesis of Condensed 2H-Pyrimidin-4-amine Libraries Under Microwave Irradiation

The novel dual use of formamide-POCl₃ mixture for the incorporation of a C-N fragment to form the pyrimidine nucleus and its subsequent chlorination in an efficient, one-pot synthesis of potentially bioactive condensed 2H-pyrimidin-4-amine libraries under microwave irradiation (MWI) is reported. The one-pot microwave-assisted synthetic protocol is high-yielding, ecofriendly, rapid, and novel as well as eliminates intermittent workups. The protocol can be adapted for the library synthesis of series of a condensed pyrimidines.     

Three-Component One-Pot Synthesis of Polyhydroacrodine Derivatives in Aqueous Media

9,10-Diaryldecahydroacridine-1,8-diones were synthesized by a three-component reaction of aromatic aldehydes, aromatic amines, and 5,5-dimethyl-1,3-cyclohexanedione using sodium 1-dodecanesulfonic (SDS) as the catalyst in aqueous media. The key intermediates before the cyclization step were obtained and characterized. The structures of all the products were determined by IR and ¹H NMR spectra and further confirmed by single-crystal x-ray diffraction analysis.     

一锅法合成甲基丙烯酰基封端的PLA-PEG-PLA大分子单体

以辛酸亚锡[Sn(Oct)2]为催化剂、聚乙二醇为引发剂引发丙交酯开环聚合,用水终止反应后再加入甲基丙烯酸酐反应即可得到甲基丙烯酰基封端的PLA-PEG-PLA大分子单体。上述两步反应可一锅进行,操作简便、收率高。采用GPC、FTIR、^1H-NMR、TG、XRD等分析手段表征了大分子单体的结构和性质。所得大分子单体的水溶液在光引发剂存在下,能被UV引发光聚合形成水凝胶。该水凝胶作为可降解生物材料可用于药物控释栽体和组织工程支架。     

New,Convenient, One-Pot Method for the Synthesis of Thiazolyl-pyrazolones from Dehydroacetic Acid Derivative via a Multicomponent Approach

A convenient one-pot method for the synthesis of thiazolyl-pyrazolones was described in excellent yields. Reaction of 3-(2-bromoacetyl)-4-hydroxy-6-methyl-2H-pyran-2-one with thiosemicarbazide and ethyl 2-(2-arylhydrazono)-3-oxobutanoates in anhydrous ethanol under reflux conditions afforded the corresponding 4-(2-arylhydrazono)-1-(4-(4-hydroxy-6-methyl-2-oxo-2H-pyran-3-yl)thiazol-2-yl)-3-methyl-1H-pyrazol-5(4H)-one in good yields. The structures of newly synthesized compounds were established on the basis of elemental analysis, infrared, ¹H NMR, and mass spectroscopic studies.     

Highly Efficient One-Pot Synthesis of 2-Aminobenzoxazoles Using Triflic Acid as a Cyclodesulfurizing Reagent

An efficient one-pot synthetic strategy for 2-aminobenzoxazoles was developed from isothiocyanates and 2-aminophenol using triflic acid as a cyclodesulfurizing reagent.

One-Pot Synthesis of Hexahydroquinolines via Hantzsch Four-Component Reaction Catalyzed by a Cheap Amino Alcohol

An economic, efficient access to hexahydroquinolines was found. In the presence of threo-(1S,2S)-2-amino-1-(4′-nitrophenyl)-1,3-propanediol, a waste product formed in the production of chloromycetin, a one-pot, four-component Hantzsch reaction of dimedone, aldehydes, ethyl acetoacetate, and ammonium acetate at room temperature furnished hexahydroquinoline derivatives in excellent yield. A possible catalytic mechanism was also suggested.     

A One-Pot Synthesis of Tetrahydro-2,5-dioxofuran-3-yl Alkylcarbamodithioates

An efficient one-pot synthesis of tetrahydro-2,5-dioxofuran-3-yl alkylcarbamodithioates via three-component reaction of maleic anhydride, CS₂, and primary amines in good yields is described.     

6-甲氧基-1,2,3,9-四氢-4H-咔唑-4-酮肟的一锅合成

报道了6-甲氧幕-1,2,3,9-四氢-4H-咔唑-4-酮肟(3b)的一锅合成法,将Fischer吲哚合成与肟化两步反应并为一步,可简化操作,提高收率.反应可以在弱碱性且温度温和的条件下一锅合成,是由于肟化使Fischer吲哚环合变得容易,羰基与肟基在互变异构方向上的差别是影响环合反应的关键因素.     

Cyanide-Free One-Pot Synthesis of Methacrylic Esters from Acetone

Methacrylic esters, represented by methyl methacrylate (MMA), are widely used as commodity chemicals. Here, the one-pot synthesis of methacrylic esters from acetone, a haloform and alcohols in the presence of an organic base is described. Using DBU as the organic base for the reaction of acetone, chloroform and methanol in acetonitrile afforded MMA in 66 % yield. When the solvent was replaced by benzonitrile, the product MMA was successfully purified by distillation. Applicability of this process to various alcohols was also investigated to show ethyl, phenyl, CF₃CH₂, and n-C₆F₁₃CH₂CH₂ esters were obtained in moderate yields. The use of bromoform instead of chloroform resulted in the improvement of the yield, for example, methyl and n-C₆F₁₃CH₂CH₂ esters up to 81 and 70 %, respectively. The reaction with deuterated starting materials acetone-d₆ and MeOH-d₄, with DBU in acetonitrile afforded deuterated MMA (MMA-d₈) in 70 % yield.     

Novel Convenient Synthesis of Mitiglinide

A novel convenient synthesis of the hypoglycemic agent mitiglinide was developed. (2S)‐4‐[(3aR,7aS)‐Octahydro‐2H‐isoindol‐2‐yl]‐4‐oxo‐2‐benzyl‐butanoic acid (6) was prepared by selective hydrolysis of ethyl 4‐[(3aR,7aS)‐octahydro‐2H‐isoindol‐2‐yl]‐4‐oxo‐2‐benzyl‐butanoate (5) using α‐chymotrypsin; the latter was prepared by a novel facile route from (3aR,7aS)‐octahydro‐2H‐isoindole. The overall yield was 25.6%.