Polyfluoroalkyl Phosphates Bearing Propargyl Substituents

Russian Journal of General Chemistry - Polyfluoroalkyl dichlorophosphates react easily with propargyl alcohol under mild conditions (22–62°С, 3 h, pyridine-toluene) to form...     

New Catalytic Synthesis of Polyfluoroalkyl Chlorosulfites

Russian Journal of General Chemistry -     

多氟烷基取代的环丙烷衍生物的合成

以连二亚硫酸钠为引发剂, 烯丙基丙二酸二乙酯与多氟烷基碘代烷在温和反应条件下反应, 方便地得到一系列多氟烷基取代的环丙烷衍生物, 产率45%～55%. 在相同条件下, 烯丙基乙酰乙酸乙酯与多氟烷基碘代烷反应得到相应的加成物, 加成物随后用碱处理也得到环合的产物.     

反丁烯二酰基桥连的带不同取代基的卟啉二联体的合成与性质

合成了反丁烯二酰基桥连的3种带不同取代基的卟啉二联体, 通过红外光谱, 紫外-可见光谱, 核磁共振波谱和质谱对化合物的结构进行了确认, 并研究了二联体的表面光电压谱, 荧光光谱和激光拉曼光谱的变化. 结果表明, 取代基的类型对卟啉二联体分子的荧光量子产率有显著影响, 带供电子基团的甲氧基增强了荧光量子产率, 而带吸电子基团的氯则降低了荧光量子产率, 并且吸电子基团的氯比供电子基团的甲氧基对荧光的影响更大. 取代基的电子效应对卟啉二联体的荧光性和激光拉曼光谱有较大影响.     

Synthesis of Octaaryl Naphthalenes and Anthracenes with Different Substituents

A synthesis of multiply arylated naphthalenes and anthracenes with eight different substituents has been accomplished. The key intermediates are tetraarylthiophene S ‐oxides, which are synthesized through a method involving sequential C−H arylation and cross‐coupling from 3‐methoxythiophene, followed by oxidation of the sulfur atom. The resulting tetraarylthiophene S ‐oxides can be converted into a tetraaryl benzynes or naphthalynes and then merged through [4+2] cycloaddition reaction with another tetraarylthiophene S ‐oxide, thereby resulting in the programmed synthesis of octaarylnaphthalenes and octaarylanthracenes.     

大基团取代不对称茂钛（Ⅳ）化合物的合成

大基团取代不对称茂钛（Ⅳ）化合物的合成舒学军贺峥杰＊陈寿山（南开大学元素有机化学研究所天津３０００７１）关键词有机锂，富烯，茂钛化合物，合成１９９６－０６－１９收稿，１９９６－１２－３１修回国家自然科学基金资助课题取代茂钛化合物常常是烯烃异构化的良好...     

Synthesis of 2,2'-Quinocyanines with Long N-Alkyl Substituents

2,2'-Quinocyanines with long alkyl substituents on one or both nitrogen atoms have been synthesized. ¹H NMR spectroscopy has been used to study the processes occurring during the alkylation of the starting quinoline bases.     

2,5-二芳基取代基-1,3,4-噁二唑类衍生物的合成与表征

以双酰肼环合法合成了含1,3,4-噁二唑结构单元的溴代芳卤,然后通过Sonogash ira钯催化偶联作用与不同单取代炔反应合成了3个新的2,5-二取代-1,3,4-噁二唑类小分子衍生物,其结构经DSC,1H NMR,IR和元素分析表征。     

Synthesis and Structure Elucidation of New Spiro Compounds with Polyfluoroalkyl and Phosphonate Ester Groups

A series of spiro compounds with polyfluoroalkyl and phosphonate ester groups has been synthesized via several steps. The structures of these compounds were confirmed by ¹H NMR,¹³C NMR, infrared (IR), and mass spectrometry (MS) as well. The possible reaction mechanism for the formation of these products was also proposed.     

Synthesis of Cyclotriphosphazenes Containing Cyanostilbenes with Different Terminal Substituents

Abstract

The synthesis and mesomorphic properties of a class of cyclotriphosphazenes containing cyanostilbene groups with different terminal substituents (-H, -CH₃, -OCH₃, -CN) are described. All the resulting compounds are characterized by ¹ Barberá , J. ; Bardají , M. ; Jiménez , J. ; Laguna , A. ; Martínez , M. P. ; Oriol , L. ; Serrano , J. L. ; Zaragozano , I. Columnar mesomorphic organizations in cyclotriphosphazenes . J. Am. Chem. Soc. 2005 , 127 , 8994 – 9002 .[Crossref], [PubMed], [Web of Science ®] , [Google Scholar]H, ¹³ An , B.-K. ; Lee , D.-S. ; Lee , J.-S. ; Park , Y.-S. ; Song , H.-S. ; Park , S.-Y. Stongly fluorescent organogel system comprising fibrillar self-assembly of a trifluoromethyl-based cyanostilbene derivative . J. Am. Chem. Soc. 2004 , 126 , 10232 – 10233 .[Crossref], [PubMed], [Web of Science ®] , [Google Scholar]C, and ³¹P NMR, matrix-assisted laser desorption/ionization time of flight, and elemental analysis. The thermal behaviors of cyclotriphosphazene derivatives are studied by the means of differential scanning calorimetry and polarizing optical microscopy. Nematic phases are observed in cyclotriphosphazenes with terminal substituents (-CH₃, -OCH₃, -CN).     

Synthesis of the Bidentate Organophosphorus Compounds with an Urea Substituents

Thiourea, S-alkyl isothiourea and guanidine 1 react with diisopropylphosphite (2) and carbon tetrachloride in the aqueous basic condition easily to give the phosphorylated product 3. S-ethyl isothiourea is a very good percursor for the synthesis of the derivatives of the phosphoryl guanidine 5.     

The Catalytic Methods of Synthesis of the Phosphorus Esters with Tertiary Polyfluoroalkyl Groups

Abstract

The phosphorylation of tertiary alcohols can be performed only in some exceptional cases. We established, that phosphorylation of tertiary fluoroalkanols H(CF₂) _nCMe₂OH (I, n = 2,4) with aryl- and polyfluoroalkyl-phosphorodicnlor-idates or aryl- and alkylphosphonic dichlorides in the presence of metal of metal salt catalysts yields chloroan-hydrides (II) and (III). When benzyl phosphorochloridates (IV) are used as phosphorylating agents, either products of phosphorylation or products of alkylation are formed depending on the nature of the substituent in the aromatic ring.     

Simple and Efficient Synthesis of 1,3-Dithioles with Pyrimidinylidene or Pyrazolylidene Substituents

Abstract

2-Pyrimidinylidene-1,3-dithioles or 2-pyrazolylidene-1,3-dithioles are prepared by a three-component condensation reaction of pyrimidine-tetraone or 1H-pyrazole-4,5-dione, carbon disulfide, and dialkyl acetylendicarboxylates in the presence of tributylphosphine.

GRAPHICAL ABSTRACT      

Synthesis and Reactivity of Hydrolysis Products of Cyclic Phosphites with Amino Substituents

Abstract

Hydrolysis of several cyclic aminophosphites are discussed and compared with that of cyclic chloro/ phenoxy phosphites. An X-ray structure of a hydrolysis product, (C₆H₁₁NH₃)⁺O^?P(O)(H)(2,2′-OC₆H₄-C₆H₄OH) has been determined.     

Synthesis of New Metal-Free and Metal-Containing Phthalocyanines with Tertiaryor Quaternary Aminoethyl Substituents

Summary.  A novel phthalodinitrile derivative carrying dimethylaminoethylsulfanyl groups at positions 4 and 5 was synthesized from 2-dimethylaminoethanethiol hydrochloride and 1,2-dichloro-4,5-dicyanobenzene. Its cyclotetramerization in the presence of 2-dimethylamino-ethanol or metal salts (CoCl₂, Zn(OAc)₂) gave metal-free or metal-containing phthalocyanines (M = Co or Zn). These phthalocyanines were converted into water soluble quaternized products by reaction with methyl iodide. The new compounds were characterized by elemental analysis, IR, NMR, and electronic spectra.     

Regioselective Synthesis of Polyfluoroalkyl Substituted 6,7‐Dihydrobenzisoxazolones

Regioselective methods for synthesis of hitherto unreported both 6,7‐dihydro‐1,2‐benzisoxazol‐4(5H)‐ones and 6,7‐dihydro‐2,1‐benzisoxazol‐4(5H)‐ones with perfluoroalkyl or halogenodifluoromethyl substituents have been developed. 3‐Polyfluoroalkyl‐6,7‐dihydro‐1,2‐benzisoxazol‐4(5H)‐ones were prepared by the cyclocondensation of 2‐polyfluoroalkanoylcyclohexane‐1,3‐diones with hydroxylamine. The regioisomeric 3‐polyfluoroalkyl‐6,7‐dihydro‐2,1‐benzisoxazol‐4(5H)‐ones were synthesized by the transformation of 2‐polyfluoroalkanoylcyclohexane‐1,3‐diones into their vinylogous chlorides, followed by the interaction of obtained crude 3‐chloro‐2‐polyfluoroalkanoyl‐2‐cyclohexen‐1‐ones with sodium azide in dimethylformamide.     

含甲基及羟基取代碲碳菁染料的合成与性能

用碘甲烷及碘乙烷与２，５，６－三甲基苯碲唑、２－甲基。５－羟基苯并碲唑反应，合成了４种苯并碲唑碘化季铵盐。进一步与原甲酸乙酯反应制得了相应的新型碲碳菁染料。测定了它们在不同溶剂中的可见吸收光谱，讨论了取代基及溶剂对最大吸收波长的影响。     

Synthesis of some Indanones having Nitrogen-containing Substituents

The title compounds have been synthesized by a Friedel-Crafts acylation-alkylation between aromatic ethers and α,β-unsaturated carboxylic acids (or esters) having nitrogen-containing substituents. Polyphosphoric acid was used as condensing agent.     

O-Polyfluoroalkylation of Phenol with Polyfluoroalkyl Chlorosulfites

Russian Journal of Organic Chemistry -