bluuebunny/crossref_metadata_2025 huggingface dataset:
Poly{[4-(hydroxy)(tosyloxy)iodo]styrene}-promoted aromatisation of Hantzsch 1,4-dihydropyridines
Authors: Li Fang-Qing , Zeng Xiao-Mei , Chen Jiang-Min
Published: December 2009

Hantzsch 1,4-dihydropyridines undergo smooth aromatisation on oxidation by poly{[4-(hydroxy)(tosyloxy)iodo] styrene} (PS-HTIB) in CH2Cl2 at room temperature to afford the corresponding pyridine derivatives in good yields. The polymeric reagent can be recycled and reused with no obvious loss of activity.
A Convenient Synthesis of 2-formyl-1,8:4,5-bis(methylenedioxy)naphthalene
Authors: Zhao Ai-Hong , Xu De-Feng , Zhuo Wen , Rao Zhen , Li Shao-Shun
Published: December 2009

2,3-Dihydronaphazarin was prepared from 1,4-dimethoxybenzene and dichloromaleic anhydride. Reaction with bromochloromethane gave 1,8:4,5-bis(methylenedioxy)naphthalene which with NBS, gave 2-bromo-1,8:4,5-bis-(methylenedioxy)naphthalene. Reaction of the Grignard derivative with DMF afforded 2-formyl-1,8:4,5-bis(methylenedioxy)naphthalene. This method had several advantages compared with the reported synthesis, including fewer steps, milder condition and higher yields.
Carbamoyl Methyl Sulfoxide Compounds of Lanthanum (III) Nitrate. Crystal and Molecular Structure of [La(NO3)3 {C6H5SOCH2CON(C4H9)2}2]
Authors: Kannan S. , Fun H.K.
Published: December 2009

Carbamoyl methyl sulfoxide compounds of lanthanum (III) nitrate of the type [La(NO3)3L2] (where L = C6H5SOCH2CON(iC3H7)2, C6H5SOCH2CON(C4H9)2 C6H5SOCH2CON(iC4H9)2) have been synthesised and characterised. The structure of the compound [La(NO3)3(C6H5SOCH2CON(C4H9)2)2] shows that the C6H5SOCH2CON(C4H9)2 bonds through both the sulfoxo and carbamoyl oxygen atoms to the lanthanum(III) nitrate and acts as a bidentate chelating ligand.
Reaction of amidrazones with 1,4-diphenylbut-2-yne-1,4-dione
Authors: El-Din Ahmed M. Nour , Aly Ashraf A.
Published: December 2009

Various (2 Z)-2-({( E)[arylamino]phenylmethylene}hydrazono)-1,4-diphenylbutan-1,4-diones are obtained during the reaction of amidrazones with 1,4-diphenylbut-2-yne-1,4-dione (DBD) in boiling ethanol.
Synthesis and Characterisation of Modified Germanium (IV) Isopropoxide with Internally Functionalised oximes: Soft Transformation of Some of These to Pure Nano-Sized Germania
Authors: Agrawal Sangeeta , Bohra R. , Nagar Meena , Raju V.S.
Published: December 2009

Reactions of [Ge(OPri)4] with internally functionalised oximes in 1:1 and 1:2 molar ratios in refluxing anhydrous benzene yielded complexes of the type [Ge(OPri)4- n{ONC(CH3)C4H3O-2} n] (1, 2); [Ge(OPri)4- n{ONC(CH3)C4H3S-2} n] (3, 4); [Ge(OPri)4- n{ONC(CH3)C5H4N-2} n] (5, 6); [Ge(OPri)4- n{ONC(H)C4H3O-2} n] (7, 8); [Ge(OPri)4- n{ONC(H)C4H3S-2} n] (9, 10); [Ge(OPri)4- n{ONC(H)C5H4N-2} n] (11, 12) (where n = 1 or 2), All the above monomeric complexes are soluble in organic solvents and have been characterised by elemental analyses and spectroscopy. Thermal and hydrolytic studies of complexes 2, 4 and 8 suggest them to be potential molecular precursors for the synthesis of pure GeO2 at low temperatures by the sol-gel technique. Powder X-ray diffraction, IR spectral studies as well as SEM images of the GeO2 indicate formation of pure nano-crystalline hexagonal (α-quartz) germania at 550°C.
A three-component reaction between trialkyl phosphites or triphenylphosphine, dimethyl acetylenedicarboxylate and N-aryl-3-hydroxynaphthalene–2-carboxamide
Authors: Anary-Abbasinejad Mohammad , Hassanabadi Alireza , Mazraeh-Seffid Manouchehr
Published: December 2009

A three-component reaction between dimethyl acetylenedicarboxylate (DMAD) and trialkyl phosphites in the presence of N-aryl-3-hydroxynaphthalene-2-carboxamide leads to dialkyl 2-(dimethoxyphosphoryl)-3-[2-hydroxy-3-(arylcarbamyl)naphthalen-1-yl] succinate in excellent yields. A similar reaction with triphenylphosphine, instead of phosphites, produces dimethyl 2-[2-hydroxy-3-(arylcarbamoyl)naphthalen-1-yl]maleates. In the absence of triphenylphosphine or phosphite, DMAD adds to N-aryl-3-hydroxynaphthalene-2-carboxamide to produce alkyl 2-(alkoxycarbonylmethyl)-4-oxo-3-aryl-3,4-dihydro-2 H-naphtho[2,3- e][1,3]oxazine-2-carboxylates in good yields.
A First Homogeneous gold(III)-Catalysed Epoxidation of Aromatic Alkenes
Authors: Li Xiao-Qiang , Li Chen , Song Fan-Bo , Zhang Chi
Published: December 2009

The first example of a homogeneous gold(III)-catalysed epoxidation of aromatic alkenes at room temperature using sodium chlorite as the stoichiometric oxidant in a homogeneous trisolvent system of 2-methoxyethanol/acetonitrile/water (volume ratio: 1/3/1) is reported. A radical-trapping experiment suggested that the reaction might proceed via a radical pathway.
Simple and Convenient Synthesis of 1,3,5-triarylbenzenes from Ketones
Authors: Hu Huanan , Zhang Anjiang , Ding Lisheng , Lei Xinxiang , Zhang Lixue
Published: December 2009

A new and efficient synthesis of a series of 1,3,5-triarylbenzenes was accomplished in good yields via the triple condensation of aryl methyl ketones promoted by thionyl chloride in anhydrous ethanol. The method is simple and convenient.
Stereoselective Synthesis of (E,E)-1-Arylseleno-Substituted 1,5-Dien-3-Ynes
Authors: Zhang Rongli , Jiang Minhua , Cai Mingzhong
Published: December 2009

Sonogashira coupling of (E)-1-iodo-2-arylselenoethylenes 1 with (trimethylsilyl)acetylene gave (E)-1-arylseleno-4-(trimethylsilyl)but-1-en-3-ynes 2, which underwent desilylation to afford (E)-1-arylselenobut-1-en-3-ynes 3 in high yields. (E,E)-1-Arylseleno-substituted 1,5-dien-3-ynes 5 could be synthesised stereoselectively via Sonogashira coupling of (E)-1-arylselenobut-1-en-3-ynes 3 with (E)-vinyl iodides 4.
Synthesis and Chemical Transformation of 2-iodomethyl-1-(phenylmethyl)-1,5,6,7-tetrahydroindol-4-ones
Authors: Mphahlele Malose J. , El-Gogary Tarek M.
Published: December 2009

2-Allyl-3-benzylamino-2-cyclohexenones undergo iodine-methanol–promoted iodocyclisation under reflux to afford products characterised by combination of NMR (1H and 13C), IR and mass spectroscopic techniques as the conjugated iodolium betaine derivatives of 2-iodomethyltetrahydroindolones. The zwitterionic nature of the products in solution and in the solid state was also confirmed by their chemical behaviour and the experimental data were corroborated by information from quantum chemical calculations.
Use of 5-methoxy, 6-methoxy and 7-methoxy-α-tetralones in the Synthesis of Diterpenes, Sesquiterpenes and Other Natural Products
Authors: Poon Po S. , Banerjee Ajoy K. , Vera William J. , Mora Henry D. , Laya Manuel S. , Bedoya Liadis , Cabrera Elvia V. , Melean Carlos E.
Published: December 2009

The transformations of 5-methoxy, 6-methoxy and 7-methoxy-α-tetralones are described. Studies on the synthesis of diterpenes veadeiroic acid 12, triptolide 18, sesquiterpenes biflorin 25, mansonone F 26, cacalol 39 and a potential intermediate for 11-deoxydaunomycinone 59 from 5-methoxy-α-tetralone 1 are discussed. Several intermediates for diterpenoid compounds and a total synthesis of phytoalexin orchinol 53 from 6-methoxy-α-tetralone 2 have been accomplished. 7-Methoxy-α-tetralone 3 has proved to be a suitable starting material for a simple and short synthesis of cadinene dihydrochloride 45.
An Efficient One-Pot Synthesis of 5-(substituted amino)-1,2,4-thia- and -oxa-diazoles
Authors: Dürüst Yaşar , Yıldırım Muhammet , Aycan Aslı
Published: December 2009

A general protocol for the synthesis of 5-(substituted amino)-1,2,4-thiadiazoles by the cyclocondensation reaction of amidoximes with N-substituted thioureas in the presence of KF/Al2O3, and of 5-(cyclohexylamino)-1,2,4-oxadiazoles with DCC in the presence of KF/Al2O3 and thiourea, is described. The structures of the new compounds were elucidated by spectroscopic and physical data, and the crystal structure determination by X-ray diffraction of three examples.
Synthesis of new 5-alkyl substituted 4-thiazolidinones utilising condensation with ethyl 2-bromo alkanoates
Authors: Klip Nalan Terzioğlu , Güzel Özlen , Gürsoy Aysel
Published: December 2009

2-[(3-Ethyl-4-oxo-3,4-dihydroquinazolin-2-yl)mercaptoacetylhydrazono]-3-alkyl/aralkyl-5-ethyl/propylthiazolidin-4-ones were synthesised by the cyclisation of 1-[(3-ethyl-4-oxo-3,4-dihydroquinazolin-2-yl)mercaptoacetyl]-4-alkyl/aralkyl thiosemicarbazides with ethyl 2-bromobutanoate or ethyl 2-bromopentanoate in the presence of anhydrous sodium acetate in anhydrous ethanolic medium. The regioisomer 2-alkyl/aralkyl 3-[(3-ethyl-4-oxo-3,4-dihydroquinazolin-2-yl)mercaptoacetylamino]-5-ethyl/propylthiazolidin-4-ones were not formed.
Indirect Detection of Hydroxyl Radicals using Spin Trapping and Gas Chromatography–Mass Spectrometry
Authors: Mistry Pritesh , Najim Nigar , Purdie Ashley , Podmore Ian
Published: December 2009

In this study, hydroxyl radicals have been converted into methyl radicals by reaction with DMSO which, following capture by the spin-trap α-[4-pyridyl N-oxide]- N- t-butyl nitrone (POBN, 1), produced a novel dimethyl product (POBN-Me2, 3) identified by GC–MS. Identification was confirmed when DMSO was replaced by a deuterated analogue (d6-DMSO).
Synthesis of Lariat Aminotriazolophanes using Carbonoxysulfide
Authors: Chande Madhukar S. , Mondkar Hemant S.
Published: December 2009

The synthesis is described of some new aminotriazolophanes based on resorcinol and glutaric acid scaffolds by cyclisation reactions between various 1,ω-dihaloalkanes and the crown precursors 1,3-bis [(4-amino-5-oxy-1, 2,4-triazole-3-yl) methyleneoxy] benzene and 1,3-bis(4-amino-5-oxo-1,2,4-triazol-3-yl) propane. The latter were synthesised using carbonoxysulfide as a reactant. The syntheses of heterophanes were carried out regioselectively and the compounds were obtained in good yields.
Synthesis of acyclo C-Nucleosides of H1-antihistaminic 4-substituted [1,2,4]triazolo[4,3-a]quinazolin-5(4H)-ones
Authors: Shawali Ahmad S. , Hassaneen Hamdi M. , Shurrab Nabil Kh.
Published: December 2009

Two series of aldose N-(3-substituted-4-oxo-3,4-dihydroquinazolin-2-yl)hydrazones were prepared by the reaction of each of the aldoses with the appropriate 2-hydrazino-3-substituted-quinazolin-4(3H)-ones. Oxidative cyclisation of these aldose hydrazones with ferric chloride in ethanol yielded the title acyclo C-nucleosides.
Extraction of Azo Dye Molecules from Aqueous Solution using Polyamidoamine Dendrimer Based Polymeric Network
Authors: Ghosh Samaresh
Published: December 2009

Synthesis of novel polyamidoamine (PAMAM) dendrimer based network polymer 2 based on the reaction between an amine-terminated PAMAM dendrimer 1 (G = 3, ethylenediamine core) and butanediol diglycidylether has been achieved. The divergent approach has been employed for the synthesis of the PAMAM dendrimer 1. This polyamidoamine (PAMAM) dendrimer based network polymer 2 has been successfully characterised by means of FT-IR spectroscopy and elemental analyses and the extraction of methyl orange dye molecules from aqueous solution has been investigated.
Stereoselective Synthesis of dialkyl 2-benzoyloxy-3-(N-alkyl-N‘-arylcarbamimidoyl)succinates: A Four Component Reaction
Authors: Anary-Abbasinejad Mohammad , Kamali-Gharamaleki Maryam
Published: December 2009

An improved four-component reaction of isocyanides is described. The reaction between alkyl isocyanides, dialkyl acetylenedicarboxylates, aromatic amines and benzoic acid in dichloromethane at room temperature leads to dialkyl 2-benzoyloxy-3-( N-alkyl- N′-arylcarbamimidoyl)succinates in good yields
Autoxidation of Organoboranes and Related Organometallics: Radicals and their Ramifications
Authors: Davies Alwyn G.
Published: December 2009

The identification, 50 years ago, of the autoxidation products of organoboranes as organoperoxyboranes, and of the mechanism of the reaction as a radical chain, has had far-reaching consequences in organometallic and organic chemistry in the identification of organic radicals and of other radical reactions, in the use of organoboron compounds in synthesis and catalysis, in the parallel chemistry of other metals (particularly, currently, of zinc), and of the behaviour of metals as hydrogen equivalents. This review traces the course of some of those developments in the radical chemistry of compounds in which oxygen forms a bond with boron and related metals, and summarises the present position.
Synthesis of Novel Cyclopentenone Derivatives and Crystal Structure Determination of 3,4-bis(4-chlorophenyl)-5,5- dimethyl-4-hydroxy-2-cyclopenten-1-one
Authors: Marjani Katayoun , Mousavi Mohsen , Ashouri Akram , Arazi Omid , Bourghani Samira , Asgari Maryam
Published: December 2009

New cyclopentenone derivatives were prepared via aldol condensation of substituted benzils with acetone derivatives in alkaline media. The structures of products were confirmed by elemental analysis, IR, 1H NMR, 13C NMR and mass spectroscopy and supported by a single crystal X-ray diffraction analysis of 3,4- bis(4-chlorophenyl)-5,5- dimethyl-4-hydroxy-2-cyclopenten-1-one. The crystal structure of title compound in the solid state is stabilised by O–H…O and C-H…O hydrogen bonds, as well as by Cl…Cl close contacts.
Phosphine-Free Cross-Coupling Reaction of Halopyridines with Arylboronic Acids in an Ionic Liquid: Water Mixture
Authors: Xin Bingwei
Published: December 2009

Palladium acetate-catalysed Suzuki reaction of halopyridines and arylboronic acids has been investigated in room-temperature ionic liquids in the absence of the phosphine ligand. A significant effect of water on the efficiency of the Suzuki reaction in ionic liquids was observed. The mixture of ionic liquid and water significantly enhanced the rate of the coupling reaction. The separation of the product was easily performed by extraction with diethyl ether and the Pd(OAc)2–[bmim][PF6] (1-butyl-3-methylimidazolium hexafluorophosphate) can be reused six times with only a small loss of reactivity.
Synthesis of 2-acetyl-7,8-dimethoxy-1,2,3,4-tetrahydronaphthalene
Authors: Vera William , Banerjee Ajoy K.
Published: December 2009

An attempt has been made to synthesise 2-acetyl-7,8-dimethoxy-1,2,3,4-tetrahydronaphthalene aiming at its transformation to intermediates for the synthesis of natural products
The Conformation of Some ortho-bromoarylaldehydes
Authors: Hanson James R. , Hitchcock Peter B. , Toche Francois
Published: December 2009

X-Ray crystallographic studies have shown that an ortho-bromo substituent has less effect on the plane of rotation of an aryl carbonyl group than on an adjacent nitro group.
Laxanol, a new 2,5-Diaryl-3,4-Dihydroxymethyltetrahydrofuran Type Lignan from Justicia Laxa
Authors: Hu Jin-Feng , Starks Courtney M. , Garo Eliane , Hough Grayson W. , Rice Stephanie M. , Goering Matt G. , O'Neil-Johnson Mark , Eldridge Gary R.
Published: December 2009

The unsymmetrical 2,5-diaryl-tetrahydrofuran type lignan, 2-(3′-methoxy-4′-hydroxyphenyl)-3,4-dihydroxymethyl-5-(3″-methoxy-5″-hydroxyphenyl)-tetrahydrofuran, laxanol (1), was obtained from Justicia laxa via high-throughput natural product chemistry methods as a mass-limited sample and its structure was elucidated by capillary scale NMR and HR-/LR-ESIMS analyses.
Syntheses of (Z)-Allyl Chlorides from Baylis–Hillman Adducts with a Trichlorotriazine/DMF System
Authors: Li Jian , Li Shaoyu , Jia Xueshun , Zhang Yongmin
Published: December 2009

Stereoselective transformation of Baylis–Hillman adducts 1 into corresponding ( Z)-allyl chlorides 2 have been achieved by treatment with 2,4,6-trichloro [1,3,5]triazine and N, N-dimethyl formamide. This novel approach proceeds readily at room temperature within a few hours with excellent yields and stereoselectivity.
Facile Diastereoselective Synthesis of Phosphonate Esters Bearing Cyclic or Acyclic Amides
Authors: Maghsoodlou Malek Taher , Charati Faramarz Rostami , Khorassani Sayyed Mostafa Habibi , Ghasemzadeh Marjan , Makha Mohamed
Published: December 2009

Phosphonate esters were obtained in excellent yields from a 1:1:1 addition reaction between triphenyl phosphite, dialkyl acetylenedicarboxylate and NH acids (maleimide, succinimide and N-phenylacetamide). The stereochemistry was established by solution NMR and single X-ray crystallography for two of the phosphonate esters. Dynamic effects of the maleimide moiety was observed and determined by 1H and 13C NMR. The free energy of activation is established for the rotation of the maleimide moiety around the N-C bond in dimethyl (2S*,3R*)-2-(2,5-dioxo-2,5-dihydropyrrol-1-yl)-3-(diphenoxyphosphoryl)butanedioate as 47 ± 2 kJ/mol.
7α-Alkoxyestra-1,3,5(10)-Trienes
Authors: Yasuda Takumi , Shima Yuji , Ideta Keiko , das Neves Oliveira Cristina , Thiemann Thies
Published: December 2009

α-Alkoxyestradiols were prepared through LiAlH4 reduction of a suitably protected 6α,7α-epoxyestra-1,3,5(10)-trien-3-ol-17-one, alkylation of the resultant 7α-hydroxyestra-1,3,5(10)-trien-3-ol-17-one derivative and subsequent transformation of the C17 functionality.
Three-Component Reaction between 3-Hydroxy-2-Naphthoic Acid, Aromatic Aldehydes and Acetonitrile in the Presence of Chlorosulfonic Acid: Synthesis of 4-(Acetylaminoarylmethyl)-3-Hydroxy-2-Naphthoic Acid
Authors: Anary-Abbasinejad Mohammad , Hassanabadi Alireza , Ghanee Fatemeh , Tahmasbnia Nahid
Published: December 2009

The one-pot, three-component reaction between 3-hydroxy-2-naphthoic acid, aromatic aldehydes and acetonitrile in the presence of chlorosulfonic acid leads to 4-(acetylaminoarylmethyl)-3-hydroxy-2-naphthoic acids in excellent yields.
Study of reaction between triphenylphosphine and activated acetylenic esters in the presence of benzanilide and some its derivatives
Authors: Hazeri Nourollah , Maghsoodlou Malek Taher , Khorassani Sayyed Mostafa Habibi , Nassiri Mahmoud , Afarini Zahra
Published: December 2009

Triphenylphosphine reacts with dialkyl acetylenedicarboxylates in the presence of NH-acids, such as benzanilide, 2-cyanobenzanilide, N-(2-acetylphenyl)benzamide, 3-nitrobenzanilide and methyl 2-benzamidobenzoate to generate stable phosphorus ylides. These stable ylides exist in solution as a mixture of two geometrical isomers as a result of restricted rotation around the carbon-carbon partial double bond resulting from conjugation of the ylide moiety with the adjacent carbonyl group.
Strontium(II) Triflate Catalysed Condensation of β-Naphthol, Aldehyde and Urea or Amides: A Facile Synthesis of Amidoalkyl Naphthols
Authors: Su Weike , Tang Wenyuan , Li Jianjun
Published: December 2009

A novel and efficient synthesis of amidoalkyl naphthols has been developed by one-pot condensation of β-naphthol, aromatic aldehydes and urea or amides in the presence of strontium(II) triflate as a catalyst in high yields.
Novel heterocyclic compounds from 2-carboxy-6-methoxybenzofuran-3-acetic acid anhydride
Authors: Patankar Jyoti A. , Khombare Rajiv T. , Khanwelkar Rahul R. , Shet Jyoti B.
Published: December 2009

2-Carboxy-6-methoxybenzofuran-3-acetic acid anhydride is utilised for the synthesis of novel polycyclic heteroaromatic compounds in which the benzofuran ring is fused or bound to pyrido[1,4]benzothiazine, thiazole, pyridine, pyrazolo-pyridine, pyrazole, pyrano-pyridine, and pyrazolo[1,5-a]pyrido[3,2-e]pyrimidines using versatile reaction strategies.
Solid state asymmetric synthesis of chiral crystals of 5- and 7-membered ring ketones
Authors: Xu Xianzhu , Wang Peng , Xia Wujiong , Yang Chao
Published: December 2009

The results of absolute asymmetric photochemical studies on 5- and 7-membered spiroketones in the solid state are described. Photolysis of 7-membered spiroketone undergoing a Norrish type II cyclisation reaction gives enantioselectivity excesses up to 93%. Irradiation of 5-membered spiroketone afforded a racemic product. The results are rationalised by the X-ray crystallographic method.
First synthesis of antitubercular natural product 2-hydroxy-5-(4-hydroxy-benzyl) benzaldehyde (Forkienin)
Authors: Singh Ashima , Sharma M.L. , Singh Jasvinder
Published: December 2009

The synthesis of 2-hydroxy-5-(4-hydroxybenzyl)benzaldehyde an antitubercular compound, from the readily available starting compound p-hydroxybenzoic acid in 4 steps is described.
Synthesis and structure of new low dimensional polymeric haloplumbate(II) complexes [Pb4Br12(C40H40N8)] and [Pb4Cl12(C40H40N8)]·H2O
Authors: Li Yinyan , Zheng Gouli , Lin Jun
Published: December 2009

New low dimensional polymeric haloplumbate(II) complexes of the dication of (4,4′-bis(imidazolyl-ylmethyl)biphenyl) were synthesised and their crystal structures determined. Complex 1, [Pb4Br12(C40H40N8)], has cis-edge-shared, octahedral, lead bromide double chains. In compound 2 [Pb4Cl12(C40H40N8)].H2O, the inorganic chains are corner-shared, square pyramidal chains of lead chloride. In both compounds the organic ammoniums form regular layers that alternate with the inorganic chains. Strong hydrogen bonds of Pb–X··HN form between the organic and inorganic components in these complexes, which are always considered as an important interaction in supramolecular syntheses. The optical properties of compound 1 and compound 2 yielded photoluminescence spectra, which are attributed to the π–π* transitions of the organic ligand.
An efficient synthesis of 3,3′-arylmethylenebis(4-hydroxy-6-methyl-2H-pyran-2-one)s in aqueous media
Authors: Sh Da-Qing , Niu Li-Hui , Yao Hao
Published: December 2009

The condensation reactions of aromatic aldehydes and 4-hydroxy-6-methyl-2H-pyran-2-one in water in the presence of sodium 1-dodecanesulfonate affords a one-pot synthesis of 3,3′-arylmethylene bis(4-hydroxy-6-methyl-2H-pyran-2-one)s.
Sodium Selenite-dimethylsulfoxide: A Highly Efficient Reagent for Dehydrogenation
Authors: Lamba Mandeep , Makrandi Jagdish Kumar
Published: December 2009

Sodium selenite in dimethylsulfoxide is a highly efficient reagent for dehydrogenation reactions and can be used under both thermal as well as microwave irradiation conditions. Using this reagent benzoins have been dehydrogenated to benzils, flavanones to flavones and 2′-hydroxy chalcones have been converted into flavones by cyclodehydrogenation.
Synthesis and Reactivity of 3-(1-hydroxy-3-buten-1-yl)chromone
Authors: Karmakar Partha , Ghosh Tarun , Chakrabarty Debasish , Maiti Sourav , Bandyopadhyay Chandrakanta
Published: December 2009

Zn-induced allylation of chromone-3-carbaldehyde 1 produces 3-(1-hydroxy-3-butene-1-yl)chromone 2, which gives back 1 on treatment with formalin under acidic conditions, and reacts differently towards nitrogenous nucleophiles.
Dipyridine Copper Chloride-Catalysed One-Pot Synthesis of (β-amino Carbonyl Compounds via Mannich Reaction
Authors: Madhav Janganati Venu , Someshwar Pola , Kumar Vanam Naveen , Rajitha Bavanthula
Published: December 2009

CuPy2Cl2-catalysed Mannich reaction of aromatic aldehyde, aromatic amine, and acetophenone proceeded smoothly in water to afford the corresponding β-amino carbonyl compounds in excellent yields.
A Fast and Convenient Coupling Reaction of Terminal Alkynes
Authors: Zhu Min , Jin Jian Chang , Tong Jian Ying
Published: December 2009

A fast and convenient coupling reaction of terminal alkynes was achieved using (diacetoxyiodo)benzene as an oxidant in the absence of palladium catalysts, providing a simple method for the synthesis of diynes in good yields in short time.
One Pot Synthesis of tetrahydroquinoline-5-thiones and Evaluation of their Antimicrobial Activities
Authors: Mourad Aboul-Fetouh E. , Aly Ashraf A. , Farag Hassan H. , Radwan Mohamed F. , Beshr Eman A.
Published: December 2009

One-pot syntheses of various tetrahydroquinoline-5-thiones are reported. The antimicrobial activity of the obtained products against various types of bacteria was estimated.
A Facile One-Pot Synthesis of 2-pyrazolyl-4-aryl-thiazoles in a Three-Component Reaction
Authors: Nalajam Guravaiah , Vedula Rajeswar Rao
Published: December 2009

A one-pot multi-component reaction of phenacylbromide, thiosemicarbazide and acetyl acetone or ethyl acetoacetate is described for the preparation of the title compounds. The key features of this methodology are its operational simplicity, mild reaction conditions, and good yields.
Solid Phase Synthesis of 4,5-disubstituted 1,2,4-triazol-3-one Derivatives from resin-bound Acylhydrazines
Authors: Liu Zhanxiang , Mu Yuanyuan , Song Zhaosheng
Published: December 2009

A new strategy for solid-phase synthesis of 4,5-disubstituted 2,4-dihydro-3 H-1,2,4-triazol-3-ones has been developed. The 4-substituted 5-(4-hydroxyphenyl)-1,2,4-triazol-3-one derivatives were synthesised from resin-bound acylhydrazines in several steps, in good overall yields and purity.
Synthesis of Some Transition Metal Complexes of Ligands Derived from 5-phenyl-2,3-dihydro-2,3-furandione
Authors: Akbas Esvet , Sonmez Mehmet , Celebi Metin , Aslanoglu Furgan
Published: December 2009

A series of amide ligands was prepared by the reactions of 5-phenyl-2,3-dihydro-2,3-furandione and aromatic amines. The ligands reacted with Cu(II) and Ni(II) ions to yield mononuclear complexes. The ligands and complexes were characterised by elemental analyses, mass, FTIR, UV-vis, 1H NMR and 13C NMR spectral studies, as well as magnetic moment, AAS and conductance measurements as appropriate
Configurational Assignment of Long-Chain Alkylated Pyridinium Aldoxime Bromides by Noesy Experiments
Authors: Sharma Mamta , Gupta A.K. , Raza S.K.
Published: December 2009

A configurational study of long-chain N-alkylated pyridinium aldoxime derivatives and their positional isomers has been carried out by two-dimensional 1H-1H NOESY (nuclear Overhauser effect spectroscopy). Cross peak intensities were observed to be enhanced with increasing mixing time. Mixing times longer than 250 ms result in increasing contribution of spin diffusion that produces unrealistic hydrogen-hydrogen distances. The results of NOE measurements showed significant enhancement in the intensity of iminyl proton resonances on irradiation of hydroxyl proton resonances and vice versa. The chemical shift difference between hydroxyl proton resonances and iminyl proton resonances was found to be ~4 ppm for syn and ~5 ppm for anti configurations. The study reveals that these compounds exist in the E configuration i.e. the syn form in solution. The syn isomer predominates; the anti isomer amounts are 3% (2-oxime), 4% (3-oxime) and 6% (4-oxime).
Alcohol Substitution and Dehydrogenation of Selenium Compounds: A Convenient Preparation of Trisubstituted Furans from allyl-substituted 1,3-dicarbonyls
Authors: Tang E , Huang Xian
Published: December 2009

Trisubstituted furans have been synthesised efficiently by an alcohol substitution and dehydrogenation reaction of selenocyclic enol ethers which were prepared by organoselenium-induced regioselective electrophilic intramolecular cyclisation of allyl-substituted 1,3-dicarbonyls.
Stereoselective Synthesis of Difunctionalised 1,3-dienes Containing Silicon and Sulfur via Palladium Catalysed Cross-Coupling Reactions
Authors: Zhang Haiyun , Ye Xinglin , Cai Mingzhong
Published: December 2009

Hydromagnesiation of alkynylsilanes 1 in diethyl ether gave ( Z)-α-silylvinyl Grignard reagents 2, which underwent a cross-coupling reaction with ( E)-α-iodovinyl sulfides 3 in the presence of Pd(PPh3)4 as catalyst to afford stereoselectively ( Z,Z)-2-silyl-3-arylsulfanyl-substituted 1,3-dienes 4 in good yields.
Synthesis of Carnitine Benzyl Esters as Prodrugs
Authors: Gong Xiao-wei , Li Jin-pei , Wu Ji-feng , Xun Li , Zhai Hai-min , Feng Bo , Xu Wen-fang , Tang Wei
Published: December 2009

The introduction of C-2 acyl groups and a benzyl ester onto L-carnitine generated a series of carnitine benzyl esters as prodrug with improved liposolubility, stability and bioavailability.
Synthesis of Pyridinium – indan-1,3-dion-2-ide Betaine Dyes and Use as Indicators of Carboxylic Acids’ Polarity
Authors: Milart Piotr
Published: December 2009

2-[4-(2,4,6-Triarylpyridinium-1-yl)phenyl]indan-1,3-dion-2-ides 5a–d, (N+C-) betaine dyes, were synthesised by reaction of 2,4,6-triarylpyrylium perchlorates 6a–d with 2-(4-aminophenyl)indan-1,3-dione 7. The solvatochromic effect of compounds 5 was investigated. The betaines obtained are suitable for polarity determination of carboxylic acids and their anhydrides.
Preparation of Pyran Derivatives Promoted by FeCl3·6H2O in Ionic Liquid
Authors: Zhang Xinying , Lv Quanjian , Fan Xuesen , Qu Guirong
Published: December 2009

The condensation reaction of chalcone and 1,3-cyclohexanedione was smoothly carried out in [bmim][BF4] with catalysis by FeCl3·6H2O. A series of substituted pyrans were obtained by this reaction, in high yields under mild conditions through a simple operational procedure. In addition, the ionic liquid together with the catalyst used can be conveniently recovered and efficiently reused.
Synthesis of Combretastatin A-4 and Erianin
Authors: Zou Yong , Xiao Chun-Fen , Zhong Rong-Qing , Wei Wen , Huang Wen-Ming , He Shu-Jie
Published: December 2009

A concise route to two anti-tubulin natural products combretastatin A-4 and erianin has been developed. Combretastatin A-4 was obtained by a Perkin reaction between 3-bromo-4-methoxyphenyl acetic acid and 3,4,5-trimethoxybenzaldehyde, hydroxyl transformation, decarboxylation with a high level of cis-selectivity ( cis/trans = 95/5), and erianin was obtained by subsequent hydrogenation. The overall yields of combretastatin A-4 and erianin were 37.5 and 30.8%, respectively.
Formation of N-acyl-N,N′-dicyclohexylureas from DCC and Arenecarboxylic Acids in the Presence of Hydroxybenzotriazole in CH2Cl2 at Room Temperature
Authors: Kaiser Carlos R. , Pinheiro Alessandra C. , de Souza Marcus V. N. , Wardell James L. , Wardell Solange M.S.V.
Published: December 2009

The syntheses of N-acyl- N,N′-dicyclohexylureas from 1,3-dicyclohexylcarbodiimide and arenecarboxylic acids [ p-XC6H4CO2H (X = H or NO2), 2-, 3- or 4-pyridinecarboxylic acid and pyrazinecarboxylic acid] in the presence of hydroxybenzotriazole in CH2Cl2 at room temperature are reported. The reactions proceed via the intermediacy of O-acyl- N,N′-dicyclohexylurea derivatives which undergo rapid O-acyl to N-acyl rearrangements. No acid anhydrides were detected. Under the same reaction conditions, the O-acyl derivative from the alkanecarboxylic acid, N-(benzyloxycarbonyl)- DL-pipecolic acid does not undergo rearrangement, as shown by the subsequent reaction with MeOH to give methyl N-(benzyloxycarbonyl)- DL-pipecolate. Characterisations were generally achieved by spectroscopic means, and specifically for N-( p-nitrobenzenecarbonyl)- N,N′-dicyclohexylurea by X-ray crystallography.
One-Pot Preparation of Ternary and Quaternary Iminium Salts from Aldehydes and Ketones
Authors: Saba Shahrokh , Vrkic Diane , Cascella Clair , DaSilva Ida , Carta Kristine , Kojtari Adeline
Published: December 2009

A facile, high-yielding, one-step procedure is described for the preparation of a wide range of stable iminium salts by direct combination of an aldehyde or a ketone with a secondary free amine in the presence of an ammonium salt. The broad scope of the method is illustrated by the preparation of iminium ions derived from aldehydes, cyclic/acyclic ketones, and cyclic/acyclic secondary amines.
Synthesis and Structures of [2.n]metacyclophane-1,2-diones
Authors: Saisyo Tatsunori , Shiino Mikiko , Shimizu Tomoe , Paudel Arjun , Yamato Takehiko
Published: December 2009

McMurry cyclisation of 1, n-bis(5-formyl-2-methoxyphenyl)alkanes afforded dimethoxy[2. n]metacyclophan-1-enes and dimethoxy[2. n]metacyclophane-1,2-diols, in which latter one was converted to dimethoxy[2. n]metacyclophane-1,2-diones by Albright–Goldman oxidation.
Synthesis and Structural Properties of Novel Polycyclic Aromatic Compounds using Photo-Induced Cyclisation of 2,7-di-tert-butyl-4-(phenylethenyl)pyrenes
Authors: Paudel Arjun , Hu Jian-yong , Yamato Takehiko
Published: December 2009

Wittig reaction of 2,7-di- tert-butylpyrene-4-carbaldehyde with benzyltriphenylphosphonium salts in the presense of n-BuLi gave 2,7-di- tert-butyl-4-(phenylethenyl)pyrenes, from which naphthalene condensed aromatic compounds, 2,7-di- tert-butyl-dibenzo[ ij, no]tetraphenes, were obtained by photo-induced cyclisation in the presense of iodine.
Three-Component One-Pot Synthesis of Unsymmetrical 1,4-dihydropyridine Derivatives in Aqueous Media
Authors: Shi Da-Qing , Yu Chen-Xia , Zhuang Qi-Ya
Published: December 2009

A series of methyl ethyl 2,6-dimethyl-4-substituted-1,4-dihydropyridine-3,5-dicarboxylates were synthesised by the three-component reaction of aldehydes, ethyl acetoacetate and methyl β-aminocrotonate in the presence of triethylbenzylammonium chloride (TEBAC) in aqueous medium. This method has the advantage of good yields.
Dioxygen Affinities and Catalytic Oxidation Performance of Unsymmetrical Bis-Schiff Base Transition-Metal Complexes with Aza-Crown Pendant Groups
Authors: Wei Xing-yue , Qin Sheng-ying
Published: December 2009

CoII and MnIII complexes with aza-crown substituted, unsymmetrical bis-Schiff base ligands have been synthesised starting from monoaza-15-crown-5 or benzo-10-aza-15-crown-5. The saturated oxygen uptakes of the CoII complexes [CoL1]–[CoL4] in diethyleneglycol/dimethyl ether solution were determined at different temperatures. The oxygenation constant ( Ko2) and thermodynamic parameters (Δ H°, Δ S°) were calculated. The MnIII complexes ([MnL1Cl]–[MnL4Cl]) were employed to catalyse styrene oxidation using molecular oxygen at ambient temperature and pressure. The modulation of O2-binding capabilities and catalytic oxidation performance by the aza-crown ether pendant groups in [ML3] and [ML4] were investigated as compared with the parent complexes [ML1] and morpholino-substituted analogue [ML2]. The results indicate that the dioxygen affinities and catalytic oxidation activities of [CoL3] and [CoL4] have been much more enhanced by aza-crown pendants. Moreover, the O2-binding capabilities of [CoL3] and [CoL4] were also improved by adding alkali metal cations (Li+, Na+ and K+) to the system, and adding Na+ shows the most significant enhancement of dioxygen affinities. Likewise, [MnL3Cl] and [MnL4Cl] exhibit the best catalytic activities: the conversion of styrene to benzaldehyde are up to 41.2% and 45.8% with more than 99% selectivity.
Synthesis of 14-aryl-14H-dibenzo[a,j]xanthene Derivatives Catalysed by Expanded Graphite under Solvent-Free Condition
Authors: Li Geng-Chen
Published: December 2009

A convenient eco-friendly procedure has been developed for the synthesis of 14-aryl-14 H-dibenzo[ a,j]xanthene derivatives by one-pot condensation of 2-naphthol and aryl aldehydes catalysed by expanded graphite under solvent-free conditions. The present methodology offers several advantages such as excellent yields, shorter reaction times, low cost and reusability of the catalyst.
Synthesis and Biological Activity of Hydrazone Derivatives Containing Pyrazole
Authors: Yang Xiao-Dong
Published: December 2009

Twelve novel hydrazone derivatives containing pyrazole rings have been prepared by condensing substituted-benzaldehyde with 2-(3,5-dimethyl- 1H-pyrazol-1-yl)acetohydrazide under microwave irradiation. Their structures were characterised by 1H NMR, IR, MS and elemental analysis. The preliminary biological activity tests showed that some of the compounds showed moderate fungicidal activity.
One-Pot Synthesis of Trans-4-Alkylthio- and 4-Arylthio-Cinnamic Acids from Trans-4-Chlorosulfonylcinnamic Acid in an Aqueous Medium
Authors: Zhang Wensheng , Kuang Chunxiang , Yang Qing
Published: December 2009

A one-pot syntheses of trans-4-alkylthio- and 4-arylthio-cinnamic acids were achieved in high yields by reduction of trans-4-chlorosulfonylcinnamic acid with stannous chloride dihydrate followed by alkylation and arylation of the resulting trans-4-thiocinnamic acid with various kinds of alkyl and activated aryl halides in an aqueous medium.
Synthesis of 2-Amino-4-Aryl-5-Oxo-4,5-Dihydropyrano[3,2-c] Chromene Derivatives Catalysed by KF-Montmorillonite
Authors: Shi Da-Qing , Wu Nan , Zhuang Qi-Ya
Published: December 2009

A series of 2-amino-4-aryl-5-oxo-4,5-dihydropyrano[3,2- c]chromene derivatives has been synthesised by the reaction of 4-hydroxycoumarin and substituted cinnamonitriles catalysed by KF-montmorillonite. The structures were characterised by IR and 1H NMR spectroscopic data and confirmed by X-ray diffraction analysis.
A Route to 4,4′-Bis(Benzocyclobutene) Based on Homocoupling Catalysed by Manganese or Iron Salts
Authors: Feng Zhiqiang , Xu Bin , Cang Hui , Wang Jintang
Published: December 2009

An efficient and practical preparation of 4,4‘-bis(benzocyclobutene) has been developed by the room temperature homocoupling of 4-bromobenzocyclobutene with magnesium and an iron or manganese catalyst.
Eudesmane-Type Sesquiterpenes from Senecio Ambraceus
Authors: Xie Wei Dong , Lai Peng Xiang , Zhao Hong , Row Kyung Ho
Published: December 2009

Investigation of the aerial parts of Senecio ambraceus afforded four eudesmane-type sesquiterpenes (1–4), of which 1 was isolated from a natural source for the first time. Its structure was established on the basis of spectroscopic methods, including IR, EI–MS, HR–ESI–MS, 1D and 2D NMR spectroscopy.
Synthesis and Cytotoxicity of Pyrrole-Amino Acid Dipeptides Containing Phosphonyl Group
Authors: Liu Ruo-yu , Ye Yong , Yang Jun-liang , Liu Cun-jiang , Zhao Yu-Fen
Published: December 2009

A series of pyrrole-amino acid dipeptide were synthesised by chloroform reaction and coupling reaction using DCC/HOBT as promoting additives. The structure of compound was confirmed by 1H NMR, 31P NMR, MS and IR. The biological activity data showed that the dipeptide containing nitrogen mustard group inhibited all four cells that were examined.
Design and Synthesis of Novel Anthranilic Diamides Containing 5,7-Dimethyl[1,2,4]Triazolo[1,5-a]Pyrimidine
Authors: Dong Wei-li , Liu Xing-hai , Xu Jun-ying , Li Zheng-ming
Published: December 2009

A new kind of anthranilic diamides containing 5,7-dimethyl[1,2,4]triazolo[1,5- a]pyrimidine were designed and synthesised. Their structures were identified by means of elemental analysis, IR, 1H NMR and MS spectra. As the key intermediate, ethyl 5,7-dimethyl[1,2,4]triazolo[1,5- a]pyrimidine-2-carboxylate (7) was synthesised by applying microwave irradiation.
Reusable Polymer-Anchored Amino Acid Copper Complex for the Synthesis of Propargylamines
Authors: Wang Liang , Cai Chun
Published: December 2009

An amino acid was anchored to chloroacetylated polystyrene beads and the polymeric ligand containing N, O donor sites was treated with a solution of CuI to form the supported copper complex. The one-pot synthesis of propargylamines was then achieved efficiently via a three-component coupling of aldehydes, alkynes and amines using the supported copper catalyst under mild conditions. The catalyst could be recovered by simple filtration and reused several times without significant loss of activity.
A Mild Highly Efficient and Green Protocol for Preparation of N-alk-2′-Enoyl Cyclic Imides Using Basic Ionic Liquid [bmIm]OH as Base and Reaction Medium
Authors: Wang Yongjiang , Mao Jianwei , Pei Wen
Published: December 2009

An efficient and green protocol for the preparation of N-alk-2′-enoyl cyclic imides at room temperature was developed using a basic ionic liquid, 1-methyl-3-butylimidazolium hydroxide, [bmIm]OH, as a base and a reaction medium.
A Synthesis of 4H-1, 4-Benzothiazines
Authors: Fu Lizhi , Xu Jinyi , Yao Hequan , Wu Xiaoming
Published: December 2009

A convenient synthesis of 4H-1, 4-benzothiazines is described. The key step is the coupling between 2-amino-5-chlorophenyl disulfide (3) and ethyl acetylenecarboxylate (4) in the presence of CuI as a catalyst or by microwave irradiation in moderate yield.
TiIV Exchanged K10-Montmorillonite: Characterisation and Catalytic Properties in Liquid-Phase Sulfide Oxidation
Authors: Khedher I. , Ghorbel A. , Fraile J.M. , Mayoral J.A.
Published: December 2009

Titanium-containing K10 has been synthesised and characterised by X-ray diffraction, UV-visible reflectance, solid state NMR spectroscopy, N2 nitrogen adsorption at 77K and chemical analysis. Two different titanium species have identified with a high dispersion in K10. The first is in an isolated penta- and hexa-coordinated state and the second is in the form of polymerised hexacoordinated species, which contains Ti-O-Ti bonds. These titanium species were found to be the catalytic sites that readily interact with oxidant to offer an active and selective catalytic system for the oxidation of sulfides. This catalytic system was studied in the asymmetric oxidation of methyl phenyl sulfide, using different types of chiral modifier, and gives excellent conversion and sulfoxide selectivity, together with a significant enantioselectivity in the range of 16–18% ee with (R)-binol.
Synthesis and Characterisation of Macrocyclic Copper(II) Complexes Containing N3O4 Donor Sets
Authors: Keypour Hassan , Dehghani-Firouzabadi Ahmad Ali , Shayesteh Maryam , Salehzadeh Sadegh
Published: December 2009

Two new macrocyclic Schiff-base complexes of Cu(II) have been prepared by the template reaction of 2,6-bis (2-formylphenoxymethyl)pyridine with 1,2-bis(2′-aminophenoxy)benzene [L1] or with 1,2-bis(2′-aminophenoxy)-4-tert-butylbenzene [L2] in the presence of Cu(II) perchlorate. The amines used have low flexibility and therefore the formation of complexes was very difficult. The synthesised 23-membered, heptadentate N3O4 complexes were characterised by elemental analysis, IR, and FAB-mass spectroscopy.
A Selenium-Catalysed Synthesis of Thiocarbamates from Nitroarenes, Carbon Monoxide and Thiols under Mild Conditions
Authors: Zhang Xiao-Peng , Lu Shi-Wei
Published: December 2009

An improved method for the selenium-catalysed synthesis of thiocarbamates under mild conditions has been developed. With acetone as solvent, the one-pot selenium-catalysed carbonylation of nitroarenes and thiols with carbon monoxide proceeds smoothly at atmospheric pressure and ambient temperature.
Reliability of π–π Stacking Interactions in Crystal Engineering: Synthesis and Structure of a Hemidirected Lead Complex
Authors: Li Tao , He Hai-bin , Jiang Mao-Sheng , Huang Ming-Jie , Cai Xiang-Yang
Published: December 2009

A new three-dimensional polymeric supramolecular PbII complex, {[Pb3(bpy)3(ip)3](H2O)}n, (bpy = 2,2′-bipyridine and ip = isophthalate), has been synthesised and characterised. Single-crystal analysis shows that {[Pb3(bpy)3(ip)3](H2O)}n contains a one-dimensional chain polymeric framework and all the Pb centres with a coordination number of six possess an electron lone pair. The coordination sphere is hemidirected which gives a highly distorted geometry. The arrangement of O- and N- atoms towards Pb atoms suggests a gap or hole in the coordination geometry around these atoms. Moreover, there are three types of π–π interactions between aromatic rings and the one-dimensional chains, which are connected by these interactions to form a three dimensional supramolecular network with the channels occupied by water molecules.
NH4Cl-Promoted Synthesis of Symmetrical and Unsymmetrical Triindolylmethanes Under Solvent-Free Conditions
Authors: Naskar Subhendu , Hazra Abhijit , Paira Priyankar , Sahu Krishnendu B. , Banerjee Sukdeb , Mondal Nirup B.
Published: December 2009

The synthesis of various triindolylmethanes from indole-3-carboxaldehyde, using indole derivatives as reactants and NH4Cl as catalyst under solvent-free conditions, is described. This methodology provides access to both symmetrical and unsymmetrical triindolylmethanes in excellent yields. With N-methylindole particularly, indole-3-carboxaldehyde appears to act as a formyl donor, leading to the exclusive formation of a symmetrically trisubstituted product. The novelty of the methodology lies in its operational simplicity, environment friendly reaction conditions, and inexpensive and easy availability of the catalyst. A plausible mechanism of formation of the products is suggested.
Synthesis of some new imidazo[3″,4″:1′,2′] pyrimido[4′,5′:4,5]thieno[2,3-c] pyridazines and other fused thieno[2,3-c]pyridazines
Authors: El-Dean Adel M. Kamal , Radwan Shaban M. , Elosealy Yasser A.
Published: December 2009

5-Amino-3,4-diphenylthieno[2,3-c]pyridazine-6-carboxamide was prepared and used as starting material to form the novel 6-chloromethyl-3,4-diphenylpyrimido[4′,5′:4,5]thieno[2,3-c]pyridazin-8(7H)-one (3), the 6-(arylaminomethyl) compounds (4a–c), 7-aryl-7,8-dihydro-3,4-diphenylimidazo[3″,4″:1′,2′]pyrimido[4′,5′:4,5]thieno[2,3-c]pyridazin-10(6H)-ones (5a–c), ethyl 7,8-dihydro-8-oxopyrimido[4′,5′:4,5]thieno[2,3-c]pyridazine-6-acetate (6) and its carbohydrazide (7). The pyridazinothienopyrimidotriazepinedione 8, pyridothienopyridazine 12 and pyridazinothienooxazepine 13 were also prepared.
New 3,7-dihydro-4H-pyrazolo[3′,4′:2,3]pyrido[4,5-d]pyrimidin-4-ones
Authors: Wang Tao , Liu Shu , Zheng Cai Hua , He Hong Wu
Published: December 2009

Thirteen novel pyrazolo[3″,4″:2,3]pyrido[4,5-d]pyrimidin-4-ones 7a–m were synthesised via tandem aza-Wittig and annulation reactions of the corresponding iminophosphoranes 5, phenylisocyanate, and substituted amine in 56–86% yields. Their structures were verified by IR, 1H NMR, EI-MS spectroscopy and elemental analysis. Preliminary bioassay indicated that some compounds possess inhibition activity against Brassica napus (rape) and Echinochloa crusgalli (barnyard grass).
Improved synthesis of 1-[hexahydrocyclopenta[c]pyrrol-2(1H)-yl]-3-(4-methylbenzenesulfonyl)urea
Authors: Qian Chao , Liu Yan , Chen Xinzhi
Published: December 2009

1-[Hexahydrocyclopenta[c]pyrrol-2(1H)-yl]-3-(4-methylbenzenesulfonyl)urea (Gliclazide) was synthesised over three steps from the starting material of cyclopentane-1,2-dicarboxylic anhydride. N-aminocyclopentane-1, 2-dicarboximide was obtained from the condensation reaction between the material and 80% hydrazine hydrate. The reduction of N-aminocyclopentane-1,2-dicarboximide and followed by the condensation with p-toluenesulfonyl urea generated Gliclazide. Every step was modified to be more simple and gave a 60% overall yield. The procedure is suitable for large-scale production.
Synthesis and photoreactions of polymethyl substituted [2.2]metacyclophanes
Authors: Paudel Arjun , Shimizu Tomoe , Yamato Takehiko
Published: December 2009

Photo-oxygenation of 4,5,6,8,12,13,14,16-octamethyl[2.2]metacyclophane using a high-pressure mercury lamp produced a mixture of mono- and bis-endoperoxides in quantitative yield, while irradiation with sunlight in chloroform afforded 1,2,3,6,7,8-hexamethyl-trans-10b,10c-dimethyl-10b,10c-dihydropyrene in 20% yield.
An unexpected dimerisation in ambient daylight
Authors: Plater M. John , Momeni Matin , Harrison William T.A.
Published: December 2009

Base catalysed condensation of indan-1,3-dione with 2-naphthaldehyde gave a mixture of the expected products 2-naphthalen-2-ylmethylene-indan-1,3-dione and a four membered ring dimer resulting from a daylight catalysed photochemical dimerisation.
Synthesis of meso-substituted porphyrins in room temparature ionic liquid
Authors: Babu Maradolla Mohan , Amaravathi Manda , Giribabu Lingamallu , Chandramouli Garimella
Published: December 2009

meso-Substituted porphyrins are synthesised from pyrrole and aryl, heteryl aldehydes cleanly and efficiently in one step by reactions at temperatures 100 °C in ionic liquid using air as oxidant.
Diene-yne cyclisation reactions of 1-ethynyl-2-vinyl-3,4-dihydronaphthalenes and 1-ethynyl-2-vinylnaphthalenes
Authors: Watanabe Masataka , Shiine Kodai , Ideta Keiko , Matsumoto Taisuke , Thiemann Thies
Published: December 2009

The reaction of 1-ethynyl-2-vinyl-3,4-dihydronaphthalenes and 1-ethynyl-2-vinylnaphthalenes over RuCl2(p-cymene) PPh3 leads to 9,10-dihydrophenanthrenes and phenanthrenes in those cases where the ethynyl group in the substrates carries a terminal proton. When 1-phenylethynyl-2-vinyl-3,4-dihydronaphthalenes or 1-phenylethynyl-2-vinylnaphthalenes are reacted over Pt(PPh3)4, 1-methylene-1H-benz[e]-4,5-dihydroindenes and 1-methylene-1H-benz[e]indenes are formed.
Rapid decomplexation of bis(thiosemicarbazonato)zinc(ll) complexes using citric acid
Authors: Holland Jason P. , Hickin Jennie A. , Grenville-Mathers Emma , Nguyen ThaoNguyen , Peach Josephine M.
Published: December 2009

Facile and quantitative dissociation of bis(thiosemicarbazonato)zinc(ll) complexes to give the corresponding neutral proligands in solution has been achieved by reaction with citric acid. This reaction provides an elegant solution to a problem encountered in the design, synthesis and purification of potential copper-based radiopharmaceuticals.