bluuebunny/crossref_metadata_2025 huggingface dataset:
Reactivity Studies on a Novel 4-(2-hydroxyphenyl)-1,3-dihydro-1,5-benzodiazepine-2-thione
Authors: Gharbi Rafik , Ben-Youssef Mouna , Martin Marie-Thérèse , Mighri Zine
Published: December 2009

The novel 4-(2-hydroxyphenyl)-1,3-dihydro-1,5-benzodiazepine-2-thione (4) has been synthesised and used as precursor to the hitherto unreported 7-methylthio[1]benzopyrano[4,3-c][1,5]-benzodiazepine (7). Hydrazinolysis of 4 gave 5-(2-aminophenylamino)-3-(2-hydroxyphenyl)-1H-pyrazole (9) which with excess of N,N-dimethylformamide dimethylacetal formed the 5-(2-hydroxyphenyl-2H-pyrazol-3-yl)-1H-benzimidazole (10).
Stereoselective Synthesis, Reactions and Antimicrobial Activity of 3-vinyl-2-azetidinones
Authors: Sharma Sain Datt , Anand Rishi Dev , Kaur Gurpreet
Published: December 2009

Stereocontrolled synthesis of 3-vinyl-2-azetidinones has been achieved by the condensation of imines and conjugated acids using phosphorus oxychloride. Transformation of these compounds to other useful intermediates has also been accomplished. Some of the compounds possess antimicrobial activity against both gram positive and gram negative bacteria.
A Facile One Step Synthesis of 3-(2-oxo-2H-chromen-3-yl)-indeno-[2,1-c]pyridazin-9-one
Authors: Rao V. Rajeswar , Kumar P. Vijaya
Published: December 2009

3-Acetylcoumarins (1) on reaction with ninhydrin (2) in acetic acid followed by treatment of in situ formed 2-hydroxy-2-[2-oxo-2-(2-oxo-2H-chromen-3-yl)-ethyl]indan-1,3-diones (3) with hydrazine hydrate resulted in the formation of corresponding 3-(2-oxo-2H-chromen-3-yl)-indeno[2,1-c]pyridazin-9-ones (4) in a single step with an excellent yields. The structures of newly synthesised compounds (4) were confirmed by unambiguous synthesis involving a two step process from 3-acetylcoumarins.
Photooxygenation of 5- and 6-chloro-1,3-cycloheptadienes and Reactions of their Endoperoxides with Base: Effects of the Chloro Substituent on the Reactions
Authors: Menzek Abdullah , Şengül M. Emin , Çetinkaya Yasin , Ceylan Selami
Published: December 2009

Photooxygenation reactions of 5- and 6-chlorocycloheptadienes 6 and 7 gave bicyclic endoperoxides 10–13. The endoperoxides 10 and 13 are major products due to the steric effects of the chloro substituent. The reactions of endoperoxide 10 with NEt3 under different conditions gave 1,4-epoxide 14, hydroxyenone 15, diketone 16, acetates 17–19 and diacetate 20. The reaction of endoperoxide 10 with pyridine and Ac2O gave diacetate 20 and dienone 21. The reaction of endoperoxide 13 with NEt3 gave tropone. The effects of the chloro substituent are discussed.
Synthesis, Characterisation and Crystal Structure of a New Bis-tripodal Ligand: N,N,N′,N′-tetrakis[(1,5-dimethylpyrazol-3-yl)methyl]-1,4-phenylenediamine
Authors: Bouabdallah Ibrahim , Ramdani Abdelkrim , Zidane Ismail , Touzani Rachid , Eddike Driss , Radi Smaail , Haidoux Abel
Published: December 2009

The synthesis of a new bis-tripodal ligand N,N,N′,N′-tetrakis[(1,5-dimethylpyrazol-3-yl)methyl]-1,4-phenylenediamine is reported and clearly established from its spectroscopic data (IR, 1H NMR, mass spectrometry) and elemental analysis. The X-ray structure of the target compound has been determined and the pyrazolyl ligand crystallises in the space group P-1 [C30H40N10; a = 7.1533(7)Å; b = 9.7541(10)Å; c = 10.7169(10)Å; α = 94.420(8)°; β = 97.920(8)°; γ = 108.088(9)°, Z = 2].
Synthesis of Symmetric Trisannelated Benzenes and 1,3,5-trimethylbenzene Using a SOCl2/EtOH Reagent
Authors: Hu Zhiguo , Dong Zhibing , Liu Jun , Liu Wenjie , Zhu Xinling
Published: December 2009

A simple and efficient method for the synthesis of symmetric trisannelated benzenes and 1,3,5-trimethylbenzene is presented. Two trisannelated benzenes and 1,3,5-trimethylbenzene were synthesised from cyclohexanone, cyclopentanone and acetone respectively in the presence of thionyl chloride in anhydrous ethanol.
An Efficient Route to Biaryl Bisbenzocyclobutene Monomers Based on Suzuki Coupling Reaction at Room Temperature
Authors: Yang Jun-xiao , Ma Kuo-yan , Zhu Fang-hua , Chen Wen , Li Bo , Zhang Lin , Xie Ru-gang
Published: December 2009

An efficient and practical preparation of the bisbenzocyclobutene monomers has been developed via the room temperature Suzuki couplings of phenyl-1, 4-diboronic ester with 4-bromobenzocyclobutene or benzocyclobutene-4-boronic acid with aryl dibromides.
Stereoselective Photochemistry of Substituted Chalcones in Solution and their Antioxidant Activities
Authors: Yaylı Nurettin , Gök Yaşar , Üçüncü Osman , Atasoy Ahmet Yaşar, Çiğdem , Şahinbaş Esra , Küçük Murat
Published: December 2009

Three new δ-truxinic type cyclobutanes [(1β,2α)-di-(4-ethylbenzoyl)-(3β,4α)-di-(4-methoxyphenyl) cyclo butane (4), (1β,2α)-di-(4-nitrobenzoyl)-(3β,4α)-di-(4-ethylphenyl) cyclobutane (5), and (1β,2α)-di-(4-ethylbenzoyl)-(3β,4α)-di-(4-ethylphenyl) cyclobutane (6)] have been prepared by stereoselective photodimerisation of the corresponding chalcone monomers (1-3) in solution. NMR and MS of the dimers are discussed. The precursor chalcones and the dimeric products showed antioxidant activities to different extents with respect to the individual compounds as well as to the antioxidant methods used.
Sulfate catalysed multicomponent cyclisation reaction of aryl isocyanates under green conditions
Authors: Dekamin Mohammad G. , Mallakpour Shadpour , Ghassemi Maryam
Published: December 2009

Sulfate anion, as a novel anionic catalyst, promotes the multicomponent cyclisation of aryl isocyantes to give heterocyclic symmetrical isocyanurates selectively under solvent-free conditions. The use of phase transfer catalysts reduces reaction times by 4-16 times.
Microwave Assisted Synthesis of N-(ethoxycarbonylmethyl)-nucleobases: Building Blocks for PNAs
Authors: Qu Gui-Rong , Li Yong , Han Su-Hui
Published: December 2009

The synthesis of N1/N9- (Ethoxycarbonylmethyl)pyrimidine/purine using as synthons for peptide nucleic acids has been described. Microwave irradiation provided the desired products by alkylation of the appropriately protected natural and substituted nucleobases with ethyl bromoacetate within 4–7 min in 48–85% yields.
A Clean One-pot Synthesis of 7-Amino-5-Aryl-6-Cyano-1,5-Dihydro-2H-Pyrano[2,3-d] Pyrimidine-2,4(3H)-Diones in Aqueous Media under Ultrasonic Irradiation
Authors: Jin Tong-Shou , Liu Li-Bin , Zhao Ying , Li Tong-Shuang
Published: December 2009

A novel approach to the synthesis of 7-amino-5-aryl-6-cyano-1,5-dihydro-2H-pyrano[2,3-d]pyrimidine-2,4(3H)-diones in aqueous media under ultrasonic irradiation without catalyst is described. This method provides several advantages such as being environmentally friendly, simple work-up procedure and milder condition. In addition, water was chosen as a green solvent.
Synthesis of 1,1-diacetates from Aromatic Aldehydes using Cerium(IV) Sulfate Tetrahydrate as Catalyst under Solvent-free Conditions
Authors: Zhang Min , Li Yi-Qun
Published: December 2009

Aromatic aldehydes can be converted into the corresponding 1,1-diacetates rapidly in the presence of catalytic amounts of Ce(SO4)2·4H2O at room temperature in excellent yield under solvent-free conditions. The catalyst can easily be recovered and reused at least 4 times.
Mechanistic Study of the Oxidation of Isonicotinate ion by Diperiodatocuprate(III) in Aqueous Alkaline Medium
Authors: Hiremath G.C , Mulla R.M , Nandibewoor S.T
Published: December 2009

The kinetics of oxidation of isonicotinate ion by diperiodatocuprate(III) (DPC) in aqueous alkaline medium at a constant ionic strength of 0.60 mol dm−3 was studied spectrophotometrically. A mechanism involving the formation of an intermediate complex between the diperiodatocuprate(III) as the oxidant species and isonicotinate ion is proposed. The reaction constants involved in the different steps of mechanism have been calculated. The activation parameters with respect to the slow step of the mechanism have been computed and discussed and thermodynamic quantities were also determined.
Synthesis, Spectroscopy and Electrochemistry of Cobalt(III) Schiff Base Complexes
Authors: Sarvestani Ali Hossein , Salimi Abdollah , Mohebbi Sajjad , Hallaj Rahman
Published: December 2009

Three Co(III) complexes of the type [Co(chel)(PBu3)]ClO4.H2O, (chel = 5-BrSalen, 5-MeOSalen and 4-MeOSalen), were synthesised and characterised by elemental analysis, IR, UV-Vis and 1H NMR spectroscopy. In their electronic spectra, the absorptions between 550 and 750 nm of these complexes are attributable to the lowest d–d transition. The axial ligands affect this transition through a σ-intraction with the dz2 orbital and the equatorial ligands affect it by π-interaction with populated d-orbitals. On the basis of an electronic structural model, in which the dz2 orbital is populated in forming cobalt(II), it is suggested that equatorial ligand substitution affects the reduction potentials less than axial ligand substitution.
Fluorine-Containing Heterocycles: Part I. Synthesis of New 7-(2-thienyl)-9-Trifluoromethylpyrido[3′,2′:4,5]Thieno[3,2-d]Pyrimidines and Related Fused Tetracyclic Systems
Authors: Bakhite Etify A. , Abdel-Rahman Abdu E. , Al-Taifi Elham A.
Published: December 2009

3-amino-6-(2-thienyl)-4-trifluoromethylthieno[2,3-b]pyridine-2-carboxamide (3) and 2-carbonitrile analogue 5 were prepared by reaction of 3-cyano-6-(2-thienyl)-4-trifluoromethylpyridine-2(1H)-thione (1) with chloroacetamide or chloroacetonitrile respectively. Heating compound 3 with triethyl orthoformate led to the formation of pyridothienopyrimidinone derivative 6. Reaction of 6 with phosphorus oxychloride produced 4-chloropyrimidine derivative 7 which underwent some nucleophilic displacements upon treatment with thiourea, piperidine, morpholine or hydrazine hydrate to give the target 4-substituted pyridothienopyrimidines 8, 10a, 10b and 11 respectively. Reaction of compound 8 with methyl iodide or ethyl chloroacetate gave compounds 9a,b. The condensation of 3-amino-6-(2-thienyl)-4-trifluoromethyl-thieno[2,3-b]pyridine-2-carbonitrile (5) with triethyl orthoformate led to the formation of methanimidate derivative 21 which upon treatment with hydrazine hydrate gave the target 3-amino-3,4-dihydro-4-imino-7-(2-thienyl)-9-trifluoromethylpyrido[3′,2′:4,5] thieno[3,2-d]pyrimidine (22). The reactions of compounds 11 and 22 with some reagents namely; triethyl orthoformate, acetic anhydride, formic acid, acetic acid, acetylacetone benzaldehyde and/or diethyl malonate were carried out and their products were identified, in most cases as [1,2,4]triazolopyridothienopyrimidines via Dimroth rearrangement.
Brand New Quantitative Solid-state Synthesis of N-pyrazolyl Azomethines
Authors: Abdel-Latif Ehab , Kaupp Gerd , Metwally Mohamed A.
Published: December 2009

Fifteen preparatively useful azomethines 3 and 5 have been quantitatively (100% yield at 100% conversion) obtained as hydrates by ball-milling together 4-aminoantipyrine 1 and 3-amino-4,6-dimethylpyrazolopyridine 4 with solid benzaldehydes 2 without passing through liquid phases. Unlike (acid catalysed) azomethine syntheses in solution, the solid–solid condensations proceed “waste free” in the absence of any auxiliaries or microwave irradiation. The product yields are quantitative in all cases and the products do not require purifying workup.
Synthesis of Caffeic Acid Esters
Authors: Xia Chun-nian , Hu Wei-xiao
Published: December 2009

A new method for the preparation of caffeic acid esters was investigated. Ten caffeic acid esters were prepared by condensation of protocatechualdehyde with malonic acid mono-esters in moderate yield. Malonic acid mono-esters were prepared from the corresponding malonate di-esters. The conformations of compounds are trans (E) form.
Uncatalysed Preparation of α-Amino Phosphonates under Solvent Free Conditions
Authors: Zahouily Mohamed , Elmakssoudi Abdelhakim , Mezdar Abdessamad , Rayadh Ahmed , Sebti Saïd
Published: December 2009

A simple, efficient and environmentally friendly procedure has been developed for the three component coupling of carbonyl compounds, aromatic and aliphatic amines and dialkyl phosphites to produce α-amino phosphonates. The α-amino phosphonates are synthesised in high yields (74–97%) in a few minutes (1–3 min) by microwave irradiation under solvent-free conditions, avoiding the use of any catalyst.
Stereoselective Synthesis of 3-azabicyclo[3,3,1]Nonan-9α-yl α-(cyclopentyl-1-ene)-α-hydroxy-α-phenylacetate Hydrochloride
Authors: Liu He , Han Xiang-Yu , Zhong Bo-Hua , Liu Ke-Liang
Published: December 2009

The isomers of α-(cyclopentyl-1-ene)-α-hydroxy-α-phenylacetic acid esters derived from 3-azabicyclo[3,3,1]nonan-9α-ol ((R)-1 and (S)-1) were obtained in high enantiomeric excess by effective stereoselective synthesis from the chiral starting material, (S) or (R)-mandelic acid using pivaldehyde as a sterically hindered reagent
Solid Phase Synthesis of Aminochalcones
Authors: Yi Fengping , Peng Yanqing , Song Gonghua , Li Jizong
Published: December 2009

A microwave-assisted solid phase synthesis of aminochalcones via the Claisen–Schmidt condensation reaction between resin-bound p-aminoacetophenone and aromatic aldehydes was described.
Parallel Synthesis of 1,2,3-triazole Derivatives on a Soluble Polymeric Support
Authors: Wang Jun-Ke , Zong Ying-Xiao , Yue Guo-Ren , Hong-Gang An , Wang Xi-Cun
Published: December 2009

The synthesis of 1,2,3-triazole derivatives on a modified soluble polymer, poly(ethylene glycol)(PEG), is described.
Vilsmeier–Haack Reaction on Hydrazones: A Convenient Synthesis of 4-formylpyrazoles
Authors: Singh Karan , Ralhan Suman , Sharma Pawan K. , Dhawan Som N.
Published: December 2009

Vilsmeier–Haack reaction has been found to be an excellent method for the formylation of a variety of hydrazones to yield the corresponding 4-formylpyrazoles.
Synthesis of Phenazone Derivatives
Authors: Moustafa Ahmed H. , Saad Hosam A.
Published: December 2009

Some new phenazone (antipyrin) derivatives 2–11 have been synthesised by acylation, alkylation, condensation and ring closure reactions of 4-aminophenazone 1. The structures of the products have been secured by elemental analyses and spectral data (IR, 1H, and 13C NMR).
A Facile Entry for Synthesis of 3-arylazo Derivatives of [1,2,4]Triazolo[4,3-a] Benzimidazole and [1,2,4]Triazolo[3,4-b]Quinazolin-5-one
Authors: Shawali Ahmad S. , Sayed Adelwahed R.
Published: December 2009

A simple synthetic strategy is described for synthesis of hitherto unreported 3-arylazo derivatives of both [1,2,4]triazolo[4,3-a]benzimidazole and [1,2,4]triazolo[3,4-b]quinazolin-5-one 6 and 7, respectively. This strategy utilises reactions of 3-chloro-1,5-diarylformazans 1 with 2-mercaptobenzimidazole 2 and 2,3-dihydro-2-thioxoquina-zolin-4(1H)-one 4 or their 2-methylthio derivatives 3 and 5, respectively. A plausible reaction mechanism is suggested for the formation of the isolated products 6 and 7.
Zn(OTf)2.6H2O catalysed acylation of aldehydes: Preparation of 1,1-diacetates and α-chloroalkyl esters
Authors: Su Weike , Can Jin
Published: December 2009

1,1-Diacetates (acylals) and α-chloroalkyl esters were prepared from carbonyl compounds with acylating reagents in the presence of 5% mol hexaaqua zinc triflate [Zn(OTf)2.6H2O] with good yields under mild reaction conditions.
Hydrolysis of amides to carboxylic acids using phthalic anhydride under microwave irradiation and solvent-free conditions
Authors: Heravi Majid M. , Zargarani Dordaneh , Shoar Rahim Hekmat , Khaleghi Shahnaz
Published: December 2009

Amides efficiently and rapidly give carboxylic acids in high yields upon reaction with phthalic anhydride under microwave irradiation in the absence of solvent.
The effects of amines on oxidative homo-coupling of terminal alkynes promoted by copper salts
Authors: Wang Lei , Yan Jincan , Li Pinhua , Wang Min , Su Caina
Published: December 2009

The effects of all kinds of amines on homo-couplings (Glaser reactions) of terminal alkynes promoted by copper salts and the Sonogashira coupling reactions were studied systematically. Diethylamine (2° amine) can serve as an excellent solvent, base and coordination ligand in the oxidative homo-coupling of terminal alkynes and several modified Glaser coupling procedures have been developed which are based on a catalytic amount of cuprous salts (CuI, CuBr or CuCl) with diethylamine systems. Homo-coupling of terminal acetylenes in the Sonogashira reaction could be inhibited by using triethylamine (3° amine) as reaction medium, and the cross-coupling products were formed as the exclusive products.
Highly efficient and stereoselective synthesis of (2Z)-2-(halomethyl)alk-2-enoates in acidic ionic liquid
Authors: Ying Taokei , Bao Weiliang , Wang Zhonghua , Zhang Yongmin
Published: December 2009

NaCl, NaBr and NaI immobilised in 1-butyl-3-methylimidazolinium hydrogen sulfate ([bmim][HSO4]) ionic liquid was found to be an efficient halogenation system for the conversion of Baylis-Hillman adducts, 3-hydroxy-2-methylenealkanoates, into (2Z)-2-(halomethyl)alk-2-enoates. To maintain high stereoselectivity the protocol provides significant improvements over existing procedures.
A facile stereoselective synthesis of (E)-2,3-disubstituted allylic alcohols via hydromagnesiation of alkylarylacetylenes
Authors: Cai Mingzhong , Xia Jun
Published: December 2009

Hydromagnesiation of alkylarylacetylenes 1 in diethyl ether gave (E)-α-arylvinyl Grignard reagents 2, which reacted with aldehydes or ketones 3 to afford stereoselectively (E)-2,3-disubstituted allylic alcohols 4 in good yields.
A new method for the preparation of 1,2-benzisoxazole-3-carboxaldehyde
Authors: Kalkote Uttam R. , Panchgalle Sharad P. , Mahakal Kumodini K. , Choudhary Suman M. , Chavan Subhash P.
Published: December 2009

Synthesis of 1,2-benzisoxazole-3-carboxaldehyde is achieved from 3-methyl 1,2-benzisoxazole via 3-ethoxymethyl-1,2-benzisoxazole (4).
Structure confirmation of L-iso-glutamine derivatives
Authors: Li Xun , Xu Wen-Fang
Published: December 2009

L-iso-glutamine derivatives as an APNIs was prepared by the condensation reaction of N-(3,4,5-trimethoxybenzoyl)-glutamic acid anhydride with L-amino acid methyl ester hydrochloride. The structure was confirmed by MS, Elemental and X-ray single crystal diffraction.
Catalytic Friedel–Crafts acylation of aromatic ethers using SmI3
Authors: Chen Xiaohang , Yu Mingxin , Wang Meijun
Published: December 2009

10% mol SmI3 catalysed the Friedel–Crafts acylation of aromatic ethers by acyl chlorides in acetonitrile with the yields of 48–82%. Reactions of various substituted aromatic ethers with acyl chloride were studied. The structures of compounds were established by IR and 1H NMR. The main product obtained with anisole is the para-substituted compound with only a trace (<5 %) of meta and ortho substituted products. This shows that the acylation of aromatic ethers is highly regioselective in the presence of SmI3, a pattern repeated with the other aromatic ethers used.
Al/Hg – mediated Reductive Dimerisation of 3-methoxycarbonyl-4-oxo-4H-1-benzopyran
Authors: Ghosh Tarun , Kumar Ranabir Sur , Bandyopadhyay Chandrakanta
Published: December 2009

Aluminium amalgam – mediated reductive dimerisation of 3-methoxycarbonyl-4-oxo-4H-1-benzopyran produced two sets of diastereomeric bichromones coupled through 2,2′ and 2,4′- positions; the latter set of diastereomers underwent diastereoconvergent dehydration to produce Z-3,3′-dimethoxycabonyl-3H-2,4′-bi[1-benzopyran-2-ylidene]-4-one.
Task-specific Ionic Liquids as Efficient, Green and Recyclable Reagents and Solvents for Oxidation of Olefins
Authors: Wang Zhiming , Wang Congna , Bao Weiliang , Ying Taokei
Published: December 2009

Two kinds of task-specific ionic liquids (Ils) composed of imidazolinium or pyridinium cations with a carboxy group and hydrogensulfate as counterion have been synthesised and their application in oxidation of olefins has been studied. The carbonyl compounds were obtained from the oxidation of chain olefins, and 1,2-cycloalkandiols were obtained from cycloalkenes in the novel oxidation systems which are easily manipulated. The products can be easily isolated from the reaction system and the ILs can readily be recovered and reused.
Synthesis of Trans-cinnamic Acids from Aryl Aldehydes and Aryl Aldehyde Bisulfite Adducts with Malonic Acid Using Piperazine
Authors: Khosropour Ahmad Reza , Khodaei Mohammad Mehdi , Moghanian Hassan
Published: December 2009

Piperazine as a new reagent for the condensation of aryl aldehydes and their bisulfite adducts with malonic acid are described which afford the corresponding cinnamic acids in excellent yields and short reaction times in the absence of solvents under microwave irradiation.
Synthesis of Carbamate Derivatives of Dibromodibenzo[d,g][1,3,6,2] Dioxathiaphosphocin 6-oxides
Authors: Babu Mesa Francis Stephen , Reddy Cirandur Suresh
Published: December 2009

6-Alkylcarbamato-2,10-dibromodibenzo[d,g][1,3,6,2]dioxathiaphosphocin 6-oxides were prepared by cyclisation of 5,5′-dibromo-2,2′-dihydroxydiphenyl sulfide with dichlorophosphinyl carbamates/thiocarbamates, obtained by the addition of alcohols/thiols to dichloroisocyanatophosphine oxide, and characterised by IR, 1H, 13C, 31P NMR and mass spectral studies.
Azoles and Azolo-Azines via 3-(3-Methylbenzofuran-2-Yl)-3-Oxopropanenitrile
Authors: Dawood Kamal M. , Farag Ahmad M. , Abdel-Aziz Hatem A.
Published: December 2009

3-(3-Methylbenzofuran-2-yl)-3-oxopropanenitrile (2), a versatile synthon, was prepared and utilised in the synthesis of several azoles and fused azolo-azine derivatives.
A Facile Stereoselective Synthesis of 1,3-dienyltellurides via Palladium Catalysed Cross-Coupling Reactions
Authors: Cai Mingzhong , Chen Junmin , Hao Wenyan
Published: December 2009

Hydrozirconation of terminal alkynes 1 gives (E)-alkenylzirconium complexes 3, which cross-couple with (E)-α-iodovinyltellurides 4 in the presence of [Pd(PPh3)4] catalyst to afford stereoselectively 1,3-dienyltellurides 5 in good yields.
Preparation and Spectroscopic Characterisation of a Series of Heterobimetallic N-phenyldiethanolaminate-alkoxide Derivatives of Oxovanadium(V)
Authors: Singh Ghadwal Rajendra , Mehrotra Ram C. , Singh Anirudh
Published: December 2009

Reaction of VO(OPri)3 with two equivalents of N-phenyldiethanolamine (PhDEAH2) yields a homometallic complex [VO(PhDEA)(PhDEAH)] 1, which reacts with a number of metal alkoxides to afford heterobimetallic oxovanadium(V) complexes of the types [VO(PhDEA)2{M(OR)n-1}] [where PhDEA = C6H5N(CH2CH2O–)2], [M =: Al (n = 3, R = Pri) 2; Al (n = 3, R = But) 3; Ti (n = 4, R = Pri) 4; Zr (n = 4, R = Pri) 5; Nb (n = 5, R = Pri) 6; Ta (n = 5, R = Pri) 7. The derivative [VO(PhDEA)(OSiPh3)] 8 has been prepared by the equimolar interaction of [VO(PhDEA)(OPri)] with Ph3SiOH. All of these complexes have been characterised by spectroscopic (IR; 1H, 13C, 27Al and 51V NMR) studies, elemental analyses, and molecular weight measurements. The derivative 2 has also been characterised by FAB mass spectral studies, which supports for its monomeric nature.
FT–IR Studies on Langmuir–Blodgett Films of Novel Phosphorus Amphiphiles: Spontaneous Polycondensation at the Air/Water Interface
Authors: Wang Hai-Yan , Li Yan-Mei , Xiao Yi , Zhao Yu-Fen , Wu Li-Xin
Published: December 2009

A series of amphiphilic N-(O,O-dihexadecyl)phosphorylamino acids were designed and synthesised, and the transmission FT–IR spectroscopic investigation of their Langmuir–Blodgett films (LB films) on CaF2 substrates indicates the spontaneous polycondensation at the air/water interface before the deposition.
N-Bromophthalimide [NBPI] as a Powerful Oxidizing Agent for the Facile and Chemoselective Oxidation of Thiols to Symmetrical Disulfides
Authors: Khazaei Ardeshir , Manesh Abbas Amini , Rostami Amin
Published: December 2009

A new application of N-bromophthalimide for the facile oxidation of thiols to their corresponding symmetrical disulfides is described. A wide variety of thiols (aromatic, aliphatic and heterocyclic) were selectively oxidised to their corresponding disulfides with [NBPI] in a mixture of acetone and water under microwave irradiation in a microwave oven at a power output of 650W.
Bromination of Endo- and Exo-benzocyclobutenonorbornene Derivatives: Neighbour Group Effect on Bromination
Authors: Uzundumlu Eren , Daştan Arif
Published: December 2009

The electrophilic addition of bromine to 13-anti-bromo-endo-benzocyclobutenonorbornene 7 at −50 ± 5 °C has led in high yield to the formation of the rearranged dibromides 9, 10 and 11. In addition to this, bromination of exo isomer 8 results in formation of rearranged 9 and non rearranged product 10. However, high-temperature bromination of endo 7 and exo isomer 8 at 77 °C gave only non-rearranged products. The possible role of a substituent in rearrangements is discussed in these systems.
A Facile Synthesis of Acylhydrazines from Acylbenzotriazoles
Authors: Wang Xiaoxia , Yu Hongping , Xu Peifang , Zheng Renwei
Published: December 2009

Acylbenzotriazoles were found to react with substituted hydrazines and aqueous hydrazine under very mild conditions, thus affording a facile synthesis of three types of acylhydrazines in moderate to excellent yields.
Synthesis of Functionalised Indoline Spiropyrans by Condensation of Indolo[2,1-b][1,3]Benzoxazines with Ortho-hydroxy-substituted Aromatic Aldehydes
Authors: Amankavičienė Virgine , Asadauskas Svajus J. , Girnienė Jolanta , Šačkus Algirdas
Published: December 2009

Condensation of 5a,6-dihydro-5a,6,6-trimethyl-2-nitro-12H-indolo[2,1-b][1,3]benzoxazine derivatives with ortho-hydroxy-substituted aromatic aldehydes afforded 1′-(2-hydroxy-5-nitrobenzyl)spiro[1-benzopyran-2,2′-indoline].
Perchloric Acid Adsorbed on Silica Gel: An Efficient Heterogeneous Reusable Catalyst for Synthesis of 1,5-benzodiazepines
Authors: Das Biswanath , Reddy Majjigapu Ravinder , Ramu Ravirala , Reddy Kongara Ravinder , Geethangili Madamanchi
Published: December 2009

The condensation of o-phenylenediamines with both aliphatic (acyclic and cylic) and aromatic ketones has been carried out to produce 1,5-benzodiazepines in high yields using perchloric acid adsorbed on silica gel as a heterogeneous catalyst. The catalyst can be recycled.
Catalytic Effect of Wet Molecular Sieve 3Å in Dry Media on Syntheses of Oximes and 1,3-dioximes
Authors: Bigdeli Mohammadali , Rahmati Abbas
Published: December 2009

A simple, efficient and eco-friendly method has been developed for the condensation of hydroxylamine hydrochloride with aldehydes, ketones and 1,3-diketones in the presence of powdered molecular sieves (3Å) as catalyst. Aldoximes, ketoximes and 1,3-dioximes were obtained in excellent yields.
New 2-aryloxy Macroheterocyclic Phosphates
Authors: Yaramapa Hari Babu , Reddy Cirandur Suresh , Maralla Venugopal , Reddy Pedaiahgari Vasugovardhana
Published: December 2009

A new class of phosphorus macroheterocycles (4a–j) has been synthesised in two steps. The reaction of 1 mole of 3,4-diamino-1,2,5-oxadiazole (1) with 2 moles of aqueous formaldehyde gave a Schiff's base which subsequently underwent addition with 2 moles of 4-t-butylphenol in 1,4-dioxane, afforded N,N-bis-(5-t-butyl-2-hydroxybenzyl)furazan-3,4-diamine (2). Cyclisation of 2 in situ with various substituted aryl phosphorodichloridates (3a–j) in the presence of Et3N in THF afforded 13-membered macroheterocycles (4a–j) containing P, N, O and C in good yields.
Phase Transfer Catalysed Synthesis of Acyldiazenes from Acylhydrazines
Authors: Niu Yong-sheng , Li Jian-ping
Published: December 2009

A two-phase catalysed dehydrogenation synthesis of acyldiazenes from acylhydrazines using 2,4,6-tri-t-butylphenol/Fe(CN)63-/NaOH is reported.
Facile Access to Condensed Arenothiophenes – Preparation of Dihydrophenanthrothiophenes and Dihydrophenanthro[1]Benzothiophenes
Authors: Watanabe Masataka , Matsumoto Taisuke , Mataka Shuntaro , Thiemann Thies
Published: December 2009

4-Bromo-3-formyl-1,2-dihydronaphthalenes undergo Suzuki cross coupling and Wittig olefination reaction in a one pot procedure. The trienes obtained can be cyclised thermally under concomitant dehydrogenation to dihydrophenanthrothiophenes and dihydrophenanthro[1]benzothiophenes. An X-ray crystal structural analysis was carried out for ethyl (E)-3-[1-(1-benzothiophen-3-yl)-3,4-dihydro-2-naphthyl]propenoate.
Regioselective Synthesis of Quinolone Antibacterials via Borate Complex of Quinolone Carboxylic Acid
Authors: Heravi Majid M. , Jaddi Zeinab S. , Oskooie Hossein A. , Khaleghi Shahnaz , Ghassemzadeh Mitra
Published: December 2009

1-substituted 7-chloro-6-fluoro-4-oxo-1,2-dihydroquinoline-3-carboxylic acids were converted to borate complexes. These compounds were treated with piperazine in presence of triethylamine to afford ciprofloxacin and norfloxacin in high yields.
Selective Oxidation of Thioureas in an Ionic Liquid by Employing an Ion-supported Hypervalent Iodine(III) Reagent
Authors: Qian Weixing , Jin Erlei , Bao Weiliang , Zhang Yongmin
Published: December 2009

Several 2,4-dialkyl-3,5-bis(arylimino)-1,2,4-thiadiazolidines were synthesised under mild conditions in good yield by the selective oxidation of N-alkyl-N'-arylthioureas by using 1-(4-diacetoxyiodobenzyl)-3-methyl imidazolium tetrafluoroborate [dibmim]+[BF4]- in ionic liquids.
Synthesis of OLED Materials of Several Triarylamines by Palladium Catalysts and Their Light Emitting Property
Authors: Yu Mingxin , Wang Meijun , Chen Xiaohang , Hong Bingbing , Zhang Xiaoyan , Cheng Chienhong
Published: December 2009

Primary aryl amines reacted with aryl halides to give the secondary aryl amines by the catalysis of [Pd(dba)2/P(t-Bu)3] at 80 °C in toluene. Secondary aryl amines reacted with 1-bromo-pyrene and 9-bromo-phenanthrene and 2,7-dibromo-9H-fluorene to afford the OLED material of aminopyrene derivatives and aminophenanthrene derivatives and diamino-9H-fluorene type by the catalysis of [Pd(OAc)2/P(t-Bu)3] at 120 °C in o-xylene. The product structures were established by 1H NMR, 13C NMR, 13C(DEPT), HRMS spectra. Physical properties were examined by UV-vis, PL and DSC spectra.
A Facile Stereoselective Synthesis of (E)-1,2-disubstituted Vinyl Sulfides via Hydromagnesiation of Alkylarylacetylenes
Authors: Cai Mingzhong , Xia Jun , Wang Pingping
Published: December 2009

Hydromagnesiation of alkylarylacetylenes 1 in diethyl ether gave (E)-α-arylvinyl Grignards reagents 2, which reacted with arylsulfenyl chlorides 3 to afford stereoselectively (E)-1,2-disubstituted vinyl sulfides 4 in good yields.
A convenient one pot synthesis of fentanyl
Authors: Gupta Pradeep Kumar , Ganesan Kumaran , Pande Ambuja , Malhotra Ramesh Chandra
Published: December 2009

Fentanyl, N-(1-phenethyl-4-piperidyl) propionanilide, was prepared by performing three successive one pot reactions at room temparature.
Investigation into Direct use of Protected 3,4-Dehydropyroglutamates in Synthesis
Authors: Moody Claire M. , Young Douglas W.
Published: December 2009

Synthesis of the 3,4-dehydropyroglutamate 5 has shown it to be unstable, forming the dimer 9 on chromatography and being too readily racemised to be considered as a useful chiral synthon.
Synthesis of Platinum Nanoparticles and Then Self-Assembly on Nafion Membrane to Give a Catalyst Coated Membrane
Authors: Tang Haolin , Luo Zhiping , Pan Mu , Jiang San Ping , Liu Zhengcai
Published: December 2009

A catalyst-coated membrane (CCM) for a proton exchange membrane fuel cell (PEMFC) with Pt loading of 2.8 μg/cm2 have been prepared by self-assembling charged Pt particles on a sulfonic acid function group, SO3-, on the membrane surface. Proton conductivity of the as-obtained CCM is 0.0932 S/cm. Half-cell polarisation showed that the self-assembled membrane is electrochemical active. Electrochemical characterisation of the self-assembled electrode showed that the Pt-PDDA nanoparticles were electrocatalytic active. The performance of self-assembled MEA with a Pt loading of 2.8 μg/cm2 achieved 2.3 mW/cm2. This corresponds to Pt utilisation of 821 W per 1 g Pt. The results demonstrated the feasibility of the formation of monolayered Pt nanoparticle structure on the membrane interface. Such a monolayered structure could offer a powerful tool in fundamental studies of polymer electrolyte systems.
A Rapid and High-yield Synthesis of Aryloxyacetyl Hydrazides under Microwave Irradiation and with Phase Transfer Catalysis
Authors: Wei Tai-Bao , Liu Hong , Li Man-Lin , Zhang You-Ming
Published: December 2009

A series of aryloxyacetyl hydrazides 4a–l were synthesised under microwave irradiation and phase transfer catalysis conditions. By the optimisation of the reaction conditions, a rapid, high-yield and efficient method for the preparation of aryloxyacetyl hydrazide was given.
Catalytic synthesis of benzimidazolyl-phenoxyacetic acid O-acetyllactosyl saccharide esters by DMAP/Et3N and antiviral activity against TMV
Authors: Chen Hong , Huang Siqing , Wen Yanmei , Li Sidong
Published: December 2009

Benzimidazolyl-phenoxyacetic acid O-acetyllactosyl saccharide esters were synthesised in good yields at room temperature using DMAP/Et3N. The compounds show better antiviral activity against tobacco mosaic virus (TMV).
Ring-opening reactions of cyclopropanes. Part 8.1 Nitrosation of donor–acceptor cyclopropanes
Authors: Cermola Flavio , Di Gioia Lucrezia , Graziano Maria Liliana , Iesce Maria Rosaria
Published: December 2009

The reaction of 2,2-dialkoxycyclopropane-1-carboxylates 1a–d and monoalkoxycyclopropane 1e with NOCl gives isoxazoline- and/or isoxazole-3-carboxylates by regioselective ring-opening at C1–C2 bond. A mechanistic interpretation suggests the intermediacy of well-stabilised dipolar species.
A simple and efficient method for the synthesis of gem-diacetates from aldehydes and ketones catalysed by gallium triiodide
Authors: Sun Peipei , Hu Zhixin
Published: December 2009

Aldehydes or ketones reacted with acetic anhydride in dichloromethane at ambient temperature to produce gem-diacetates in good to excellent yields in the presence of gallium triiodide, which was generated in situ from gallium and iodine. This catalyst was also useful for the deprotection of carbonyl compounds in the presence of water.
Intermolecular double Michael reaction to construct 4-benzyl-5-imino-3-phenyl-6-oxa-1-aza-tricyclo[6.2.2.02,7]dodec-2(7)-ene-4-carbonitrile
Authors: Zoorob Hanafi H. , Hamama Wafaa S. , El-Magid Osama M. Abd , Soliman Mamdoh S.
Published: December 2009

1-azabicyclo[2.2.2]octan-3-one. HCl (1) reacts with ylidene nitrile through photo- thermal reaction conditions to give 4-benzyl-5-imino-3-phenyl-6-oxa-1-aza-tricyclo[6.2.2.02,7]dodec-2(7)-ene-4-carbonitrile. (3) via intermolecular double Micheal reaction, whereas, 5-imino-3-phenyl-6-oxa-1-azatricyclo[6.2.2.02,7]dodec-2(7)-ene-4-carbonitrile (4) was achieved via thermal conditions only.
Synthesis and some novel reactions of 8-chloro-2H-[1,2,4]triazino[3,4-b] [1,3]benzothiazole-3,4-dione and 6-chloro-2-hydrazino-1,3-benzothiazole
Authors: Kuberkar Sharad V. , Bhosale Vijay N. , Vartale Sambhaji P. , Badne Santosh G.
Published: December 2009

3,8-Dichloro-4H-[1,2,4]triazino[3,4-b][1,3]benzothiazole-4-one on reaction independently with sodium hydroxide solution and sodium azide undergo novel ring contraction reactions to give 7-chloro[1,2,4]triazolo[3,4-b][1,3] benzothiazole and 8-chloro tetrazolo[1′,5′:1,5][1,2,4]triazolo[3,4-b][1,3]benzothiazole respectively.
An efficient synthesis of an optically active (-)-(3R, 4R, 5R)-4-(1-hydroxyl-isopropyl)-3-acetyloxyl-butyrolactone
Authors: Wang JinXin , Zhang ChaoXin , Li Ying , You QiDong
Published: December 2009

An optically active β-hydroxyl–γ-butyrolactone was synthesised from nonchiral starting material by employing reductive cleavage reaction, Sharpless asymmetric epoxidation and dihydroxylation as key steps. This strategy can be used to prepare many chiral β-hydroxyl–γ-butyrolactone analogues. The crystal structure of 10 was determined by X-ray crystallographs.
Synthesis of vinyl bromides from the reaction of α, β-unsaturated carboxylic acids with ionic liquid [bmim][Br3]/[bmim]Br
Authors: Wang Congna , Bao Weiliang , Zhang Xiaoyin
Published: December 2009

Reaction of aryl α, β-unsaturated carboxylic acids with ionic liquid [bmim][Br3]/[bmim]Br affords vinyl bromides in a short reaction time and in good to excellent yields.
Williamson reaction in [bmim][BF4]: Clean and facile synthesis of aryl benzyl ethers
Authors: Wen Xinmin
Published: December 2009

1-Butyl-3-methylimidazolium tetrafluoroborate ([bmin][BF4]) has been demonstrated to be a suitable reaction medium for the synthesis of aryl benzyl ethers by the Williamson reaction. A variety of phenols react with benzyl chloride in [bmim][BF4] to afford the desired ethers in satisfactory yields. The reaction proceeds cleanly and the use of the ionic liquid allows for easy product isolation.
A Novel Synthesis of Unsymmetrical Selenides via the Cleavage of Se–se Bond by Sm/cat.CoCl2 System
Authors: Chen Rener , Su Weike , Zhong Weihui
Published: December 2009

Promoted by Sm/cat. CoCl2 system, the Se–Se bond of diaryldiselenides was easily cleaved to form a “living” intermediate, which reacted readily with alkyl halides to afford unsymmetrical alkylarylselenides in good yields under mild and neutral reaction conditions.
A green procedure for the synthesis of cinnamate esters using Aliquat®336
Authors: Mahapatra Tanusri , Patra Amarendra , Mitra Alok Kumar
Published: December 2009

As an effective solid-liquid phase-transfer catalyst as well as an ionic liquid medium Aliquat® 336 has been applied in the synthesis of cinnamate esters under mild green chemistry procedures involving microwave irradiation.
Synthesis and Structural Elucidation of Novel Spiropyrazolines Precursors to Spiro-gem-dimethylcyclopropanes
Authors: Ali Karim Ben , Boukamcha Najeh , Khemiss Abdelkader , Martin Marie-Thérèse
Published: December 2009

1,3-dipolar cycloaddition reaction of 2-diazopropane (DAP) 1 with 2-arylidene-1-tetralone 2a–b led exclusively to spiro-Δ1-pyrazolines 3a–b. When 4-methyl-2-arylidene-1-tetralones 2c–d was used as starting dipolarophile a mixture of diastereiosomeric cycloadducts 4a–b and 5a–b was obtained. The photochemical nitrogen-extrusion studied for spiropyrazolines 3a–b and 4a–b led stereospecifically to spiro-gem-dimethylcyclopropanes. In all cases, the reaction regiochemistry and stereochemistry was discussed on the basis of 2D-NMR experiments.
Ab Initio Study of Geminal Steric Hindrance Effects on the Stability of Conformations of Cyclohexane Derivatives
Authors: Nori-Shargh Davood , Amini Mostafa Mohamadpour , Jafari Maryam , Deyhimi Farzad , Jameh-Bozorghi Saeed
Published: December 2009

Ab initio and density functional theory methods (HF/3-21G*//HF/3-21G*, MP2/3-21G*//HF/3-21G*, B3LYP/3-21G*//HF/3-21G*, B3LYP/LANL2DZ*//HF/LANL2DZ*, MP2/LANL2DZ*//HF/LANL2DZ* and HF/LANL2DZ*//HF/LANL2DZ*) used to investigate the conformational properties of cyclohexane, 1,1-dimethylcyclohexane, 1,1-di-tert-butylcyclohexane, 1,1-bis(trimethylsilanyl)cyclohexane, 1,1-bis(trimethylgermanyl)cyclohexane and 1,1-bis(trimethylstannyl)cyclohex ane showed that the energy difference between the chair and twist-boat conformations and also the ring flipping energy barrier decreases from cyclohexane, 1,1-dimethylcyclohexane to 1,1-di-tert-butylcyclohexane, and increases from 1,1-bis(trimethylsilanyl)cyclohexane, 1,1-bis(trimethylgermanyl)cyclohexane to 1,1-bis(trimethylstannyl)cyclohexane.
Poly(vinylpyrrolidone)-bromine Complex; a Mild and Efficient Reagent for Selective Bromination of Alkenes and Oxidation of Alcohols
Authors: Lakouraj Moslem Mansour , Tajbakhsh Mahmood , Mokhtary Masoud
Published: December 2009

Poly(vinylpyrrolidone)-bromine complex (PVP–Br2) is easily prepared and used as a mild and convenient reagent for selective bromination of alkenes and at the position α-hydrogen of active carbonyl compounds. Selective oxidation of benzylic alcohols in the presence of aliphatic alcohols were also achieved at room temperature.
The Synthesis of 2-(1,2,3-Triazol-2-yl)-1,8-Naphthyridines under Microwave Irradiation
Authors: Mogilaiah Kaleru , Prashanthi Mullangi , Kavitha Siddoju , Reddy Nagavelli Vasudeva
Published: December 2009

An efficient and convenient method is described for the synthesis of 3-aryl-2-(4,5-dimethyl-2H-1,2,3-triazol-2-yl)-1,8-naphthyridines (4) from α-acetylacetaldoxime 3-aryl-1,8-naphthyridin-2-ylhydrazones (3) in the presence of acetic anhydride and DMF using basic alumina as solid support under microwave irradiation.
KHSO4 Catalysed Pechmann Condensation Under Solvent-free Conditions
Authors: Qian Jinhua , Suo Jishuan
Published: December 2009

KHSO4 is used as an alternative to conventional acid catalysts in the Pechmann condensation of phenols with β-ketoesters leading to the formation of substituted coumarins. The method is simple, cost-effective, solvent-free and gives good isolated yields.
Synthesis of 1,2,4-triazolo[4,3-a][1,8]Naphthyridines using Chloranil under Microwave Irradiation
Authors: Mogilaiah Kaleru , Rani Janapatla Uma , Sakram Boda
Published: December 2009

A simple and highly efficient procedure has been described for the synthesis of 1-aryl-4-[p-bromophenyl)-1,2, 4-triazolo[4,3-a][1,8]naphthyridines (8) by the oxidation of the corresponding aryl aldehyde 3-(p-bromophenyl)-1, 8-naphthyridin-2-ylhydrazones (7) with chloranil under microwave irradiation. The products are obtained in good yields and in a state of high purity.
Synthesis and Dynamic NMR Study of Fluorinated Dialkyl 2-[(tert-butylimino)-methylene]-3-[(2-alkoxy-2-oxoacetyl)-2-fluoroanilino]-succinates
Authors: Yavari Issa , Nasiri Farough , Djahaniani Hoorieh , Bijanzadeh Hamid R.
Published: December 2009

The 1:1 adduct produced in the reaction between tert-butyl isocyanide and dialkyl acetylenedicarboxylates was trapped by alkyl 2-fluoro-anilino-2-oxo-acetates or ethyl 2-oxo-2-(trifluoromethylanilino)-acetate to produce functionalised ketenimines in good yields. Dynamic NMR effects were observed in the 1H NMR spectra of these compounds as a result of restricted rotation around the single bond linking the aryl group to the ketenimine system. The free energy of activation (ΔG≠) for this process is 64.9–66.5 kJ mol−1.
Preparation and spectroscopic study of 13-substituted 2,11-dithiahexahydro[3.3]paracyclophanes
Authors: Lin Shaw-Tao , Yang Ya-Chen , Lin Shu-Farn , Hwang Lih-Jiun
Published: December 2009

A series of 13-substituted 2,11-dithiahexahydro[3.3]paracyclophanes each containing a substituent on the benzene ring were prepared for 1H NMR and X-ray diffraction analyses. The benzene ring and the cyclohexane ring demonstrate shielding of the hydrogen(s) of the opposite ring. The benzene ring is distorted by the substituent on that ring.
A facile and green preparation of 2,4-diarylpolyhydroquinolines
Authors: Hu Xueyuan , Zhang Xinying , Fan Xuesen , Qu Guirong , Li Yanzhen
Published: December 2009

An efficient and environmentally benign procedure for the preparation of 2,4-diarylpolyhydroquinoline derivatives from 5,5-dimethylcyclohexane-1,3-dione, chalcones and ammonium acetate under microwave irradiation in a solvent-free manner is described in this paper.
(Chloromethylene)Dimethylammonium Chloride: A Highly Efficient Reagent for the Synthesis of β-Lactams from β-Amino Acids
Authors: Kanwar Seema , Sharma Sain D.
Published: December 2009

(Chloromethylene)dimethylammonium chloride 1, is a unique reagent that conveniently and efficiently mediates the amide bond formation in β-lactams via cyclodehydration of β-amino acids leading to β-lactam formation. The process involves the formation of a highly reactive activated ester of a β-amino acid which gets cyclised to the corresponding β-lactam in excellent yield. The reaction proceeds smoothly and cleanly as the by-products formed are the water soluble-dimethyl formamide and triethylamine hydrochloride.
Biginelli condensation of aliphatic aldehydes catalysed by zinc methanesulfonate
Authors: Wang Min , Jiang Heng , Wang Zhichang
Published: December 2009

Three-component condensation of an aliphatic aldehyde, 1,3-dicarbonyl compound and urea proceeds efficiently in absolute ethanol under refluxing temperature using zinc methanesulfonate as a catalyst to afford corresponding 3,4-dihydropyrimidinone. The catalyst can be reused for several times without distinct decrease in reaction yields. The procedure is very useful for the synthesis of dihydropyrimidinones with a wide range of aliphatic aldehydes.
A practical and rapid synthesis of 2-aryloxymethylene-6-arylimidazo [2,1-b][1,3,4]thiadiazole in aqueous media
Authors: Wang Xi-Cun , Wang Man-Gang , Yang Zhi , Quan Zheng-Jun , Wang Fang , Li Zheng
Published: December 2009

A practical and rapid procedure is reported for the synthesis of a variety of 2-aryloxymethylene-6-arylimidazo[2,1-b][1,3,4]thiadiazole 3a–m by condensation reaction of 2-amino-5-aryloxymethylene-1,3,4-thiadiazole 1a–g with ω-bromoacetophenone derivatives 2a–b in aqueous media under microwave irradiation and yielded a series of novel compounds. The procedure is simple and the yields are good to excellent.
A facile synthesis of stable heterocyclic fused ring phosphorus ylides
Authors: Maghsoodlou Malek Taher , Hazeri Norollah , Khorasani Sayyed Mostafa Habibi , Afshari Ghafar , Nassiri Mahmoud
Published: December 2009

Stable crystalline phosphorus ylides were obtained in excellent yields from the 1:1:1 addition reaction between triphenylphosphine, dialkyl acetylenedicarboxylates, and strong NH-acids, such as 7-azaindole. These stabilised phosphoranes exist 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.
Simple amidation of unprotected phenol-containing 2-alkenoic acids
Authors: Morais Goreti Ribeiro , Watanabe Masataka , Tanaka Yasuko , Thiemann Thies
Published: December 2009

A series of amides of 2-E-alkenoic acids have been synthesised through the activation of these acids with dicyclohexylcarbodiimide / pentafluorophenol and further reaction with amines under microwave irradiation. In daylight, the E-configured amides undergo a slow photochemical E/Z-isomerisation. Photoirradiation experiments with selected 3-(hydroxyphenyl)-2(E)-alkenamides were carried out using a high pressure mercury UV lamp.
Synthesis of pyrano and furanoquinolines using silica chloride or amberlyst-15 as a heterogeneous catalyst
Authors: Das Biswanath , Reddy Majjigapu Ravinder , Holla Harish , Ramu Ravirala , Venkateswarlu Katta , Rao Yerra Koteswara
Published: December 2009

The coupling of three components, anilines, benzaldehydes and 3,4-dihydro-2H- pyran or 2,3-dihydrofuran to prepare the corresponding pyrano or furanoquinolines has been achieved efficiently using silica chloride or Amberlyst-15 as a heterogeneous catalyst. Amberlyst-15 can be recovered and reused.
Pinacol coupling of aromatic aldehydes mediated by TiCl3–Mn–EtOH under ultrasound irradiation
Authors: Li Ji-Tai , Chen Yan-Xue , Chang Rui-Xiang , Li Tong-Shuang
Published: December 2009

Pinacol coupling of aromatic aldehydes and ketones by TiCl3–Mn–EtOH under ultrasound irradiation can lead to the corresponding pinacols in 16–86% yields at room temperature.
Synthesis, characterisation and crystal structure of 1,2-bis(6-methylpyridin-2-yl)ethene-1,2-diol
Authors: Percino M. Judith , Chapela Víctor M. , Rodríguez-Barbarín Cecilia
Published: December 2009

From the condensation reaction of (6-methylpyridin-2-yl)methanol and pyridine-2-carbaldehyde at 130 °C without catalyst or solvent was isolated an unexpected compound 1,2-bis(6-methylpyridin-2-yl)ethene-1,2-diol, in crystal form. The new compound was characterised by mass spectroscopy, IR, 1H NMR, UV-Vis and single crystal X-ray diffraction showing that it is a symmetrical molecule with two intramolecular hydrogen bonds. The molecular and crystalline structure of 1,2-bis(6-methylpyridin-2-yl)ethene-1,2-diol indicated that the molecule crystallised in a monoclinic crystal system and belongs to P21/c space group with two molecules per unit cell. Within the accuracy of the analysis the molecule is planar and there are two moderate intramolecular O–H⃛N hydrogen bonds. We think that the presence of two moderate intramolecular hydrogen bonds gives stabilisation to the crystal structure, making isolation of a single crystal form possible.