三苯基锡与邻氨基苯甲酸型Schif碱配合物的合成及表征

合成了两种新的三苯基锡与邻氨基苯甲酸型Ｓｃｈｉｆ碱的配合物，经元素分析、ＵＶ、ＩＲ、１ＨＮＭＲ测定，对其结构进行了表征。结果表明，两种配合物具有不同的结构。在三苯基锡与水杨醛缩邻氨基苯甲酸Ｓｃｈｉｆ碱的配合物中，锡原子是六配位的，存在着酚羟基氧和亚氨基氮与锡的配键。在三苯基锡与２－羟基－１－萘醛缩邻氨基苯甲酸Ｓｃｈｉｆ碱的配合物中，锡原子是五配位的，酚羟基氧和亚氨基氮均未与锡配位，但存在着羰基氧与锡的配键     

Fused deposition modeling-based additive manufacturing (3D printing): techniques for polymer material systems

While the developments of additive manufacturing (AM) techniques have been remarkable thus far, they are still significantly limited by the range of printable, functional material systems that meet the requirements of a broad range of industries; including the health care, manufacturing, packaging, aerospace, and automotive industries. Furthermore, with the rising demand for sustainable developments, this review broadly gives the reader a good overview of existing AM techniques; with more focus on the extrusion-based technologies (fused deposition modeling and direct ink writing) due to their scalability, cost efficiency and wider range of material processability. It then goes on to identify the innovative materials and recent research activities that may support the sustainable development of extrusion-based techniques for functional and multifunctional (4D printing) part and product fabrication.     

Microwave Promoted and Improved Thermal Synthesis of Spiro[Indole‐Pyranobenzopyrans] and Spiro[Indole‐Pyranoimidazoles]

Spiro[indole‐pyranoimidazoles] ( 5 ) and spiro[indole‐pyranobenzopyrans] ( 6 ) are readily synthesized in one step in 86–92 and 91–97% yields by the Michael condensation of 3‐dicyanomethylene‐2H‐indol‐2‐ones ( 2 ) with 1‐phenyl‐2‐thiohydantoin ( 3 ) and 4‐hydroxy‐2H‐1‐benzopyran‐2‐one ( 4 ), respectively, without using any catalyst under different reaction conditions (conventional heating and microwave irradiation using (a) polar solvents (b) neutral alumina/silica gel as inorganic solid support in solvent free conditions). 2 was synthesized in situ by the Knoevenagel condensation of indole‐2,3‐dione ( 1 ) and malononitrile in the absence of any catalyst. 100% conversion was observed in most cases on TLC which also showed the formation of a single product. The comparison between the various methods is established.     

Palladium-catalyzed stereoselective intramolecular cyclization and Suzuki coupling of N-arylsulfonyl-α-chloroenamides promoted by a γ-hydroxy group

The Suzuki reaction of both (E)- and (Z)-α-chloro-γ-hydroxyenamides with benzeneboronic acid by using Pd₂(dba)₃, tBu₃P, and Cs₂CO₃ proceeded stereoselectively to afford only (E)-trisubstituted enamides. Also, palladium-catalyzed intramolecular cyclization of (E)- and (Z)-α-chloro-γ-hydroxyenamides bearing an N-arylsulfonyl group took place stereoselectively to give the corresponding (E)-2,3-dihydrobenzoisothiazole 1,1-dioxides. The γ-hyroxy group in α-chloroenamides was found to accelerate the present palladium-catalyzed carbon-carbon bond forming reactions.     

Determination of Amino Acidsas Their N-Hydroxy-succinimidyl-3-indolylacetate Derivatives by Reversed-phase HPLC

ＤｅｔｅｒｍｉｎａｔｉｏｎｏｆＡｍｉｎｏＡｃｉｄｓａｓＴｈｅｉｒＮ┐Ｈｙｄｒｏｘｙ┐ｓｕｃｃｉｎｉｍｉｄｙｌ┐３┐ｉｎｄｏｌｙｌａｃｅｔａｔｅＤｅｒｉｖａｔｉｖｅｓｂｙＲｅｖｅｒｓｅｄ┐ｐｈａｓｅＨＰＬＣ＊ＱＩＵＰｅｉ－ｈｏｎｇ＊＊（Ｄｅｐａｒｔｍｅ...     

Syntheses of 5‐(3‐Arylsydnon‐4‐yl)Tetrazole Derivatives

3‐Arylsydnone‐4‐carbohydroximic acid chlorides ( 1 ) could react with sodium azide to produce the corresponding 3‐arylsydnone‐4‐carbazidoximes ( 2 ), but not 1‐hydroxytetrazoles 3 . Treatment of 3‐arylsydnone‐4‐carbazidoximes ( 2 ) with acid chlorides such as acetyl chloride ( 4a ), propionyl chloride ( 4b ) and benzoyl chloride ( 4c ) in the presence of excess triethylamine generated the derivatives of the azidoximes 5 . To obtain the desired tetrazoles, the azidoximes 2 should first cyclize directly with acetyl chloride ( 4a ) or propionyl chloride ( 4b ) to afford the acetyl or propionyl derivatives 6 . The cyclized tetrazole derivatives 6 underwent deacylation upon heating in ethanol to give 1‐hydroxy‐5‐(3‐arylsydnon‐4‐yl)tetrazoles ( 3 ).     

鱼心中新的4—羟基—2—羟甲基—2—十七烷基—1,5—戊内酯的研究

从鳙鱼（Ａｒｉｓｔｉｃｈｔｈｙｓｎｏｂｉｌｉｓ）的心脏肌肉中分离得到一种带长链的六环内酯化合物，熔点６２．３～６２．８℃，由１ＨＮＭＲ，１３ＣＮＭＲ，ＩＲ，ＭＳ等波谱数据推导其化学结构为４羟基２羟甲基２十七烷基１，５戊内酯，文献检索表明为新化合物。     

A New and Efficient Synthesis of the HMG‐CoA Reductase Inhibitor Pitavastatin

A new synthetic method for the preparation of pitavastatin is described. The approach circumvents various synthetic problems associated with the buildup of the 3,5‐dihydroxy‐C₇ acid side chain of HMG‐CoA reductase inhibitors (statins). The use of the C₆‐amide derivative 5 instead of ester derivatives in the coupling reaction with carboxaldehyde 8 (Scheme 3) prevents undesired side reactions, such as eliminations and retro‐aldol reactions. The method provides synthetic statins, such as pitavastatin, in >99% ee and exceptionally high overall yield. The enantiomerically pure starting material, (3S)‐3‐{[(tert‐butyl)dimethylsilyl]oxy}‐5‐oxo‐5‐{[(1S)‐1‐phenylethyl]amino}pentanoic acid ( 3c ), is prepared by an improved procedure from 3‐{[(tert‐butyl)dimethylsilyl]oxy}glutaric anhydride ( 1 ) and (1S)‐1‐phenylethylamine ( 2c ; Scheme 1).     

Fenton反应产生的羟自由基及其清除的电化学方法测定

建立了一种新的测定羟自由基的电化学方法，Fenton反应产生的羟自由基氧化二甲亚砚（DMSO）生成的甲醛与乙酰丙酮、氨发生Hantzsch反应，产物3，5－二乙酰基－1，4－二氢吡啶在－1．20V（vs SCE)处有一灵敏的二阶导数极谱波，通过峰电流变化可间接测定羟自由基；拟定的方法测定了数种清除剂与羟自由基反应的反应速率常量和清除羟自由基的IC50；该法简便可靠，对于抗氧化剂的筛选具有一定的应用价值。