bluuebunny/crossref_metadata_2025 huggingface dataset:
Iron and Manganese (III) – Porphyrins as New Applicable Catalysts for Selective Oxidation of Imines with Urea–hydrogen Peroxide
Authors: Karami Bahador , Montazerozohori Morteza , Moghadam Majid , Farahi Mahnaz
Published: December 2009

A variety of imines were oxidised with urea–hydrogen peroxide using iron(III) and manganese (III)- tetraphenylporphyrins [Fe(TPP)Cl], [Mn(TPP)Cl] and manganese (III)-octabromotetraphenyl porphyrin [Mn(TPPBr8)Cl] as catalysts. Experimental results showed the released urea from UHP acts as an axial ligand. These catalysts showed high selectivity in oxidation of imines to corresponding nitrones and oxaziridines at 0°C to room temperature.
Behaviour of 3(3-indolylmethylene)-5-aryl-2(3H)-furanones as Alkylating Agents: Intra- Versus Inter-Molecular Alkylation
Authors: Abou-Elmagd Wael S.I.
Published: December 2009

5-Aryl-3-(3-indolylmethylene)-2(3 H)-furanones (6a–c) were prepared as a mixture of ( E) and ( Z) stereoisomers by condensing indole-3-carboxaldehyde with 3-aroylpropanoic acids using thionyl chloride in N,N-dimethylformamide as cyclodehydrating agent. The reaction of the furanones 6a and 6b with anhydrous aluminium chloride in benzene, toluene or anisole led to the formation of 4,4-diaryl-1-(3-indolyl)buta-1,3-diene-2-carboxylic acids (7) as mixtures of geometrical ( E, E- and E, Z-) stereoisomers via an intermolecular alkylation mode. The furanone 6c under the same reaction conditions gave 1-(4-methoxyphenyl)carbazole-3-carboxylic acid (8) via intramolecular alkylation. This represents a novel method for the synthesis of carbazole derivatives.
A General approach to Difunctionalised 1,3-dienes containing Silicon and Halogen via Hydrozirconation of (Z)-3-(trimethylsilyl)alk-3-en-1-ynes
Authors: Ye Xinglin , Wang Pingping , Cai Mingzhong
Published: December 2009

Sonogashira coupling of ( E)-α-iodovinylsilanes 1 with (trimethylsilyl)acetylene gave ( Z)-1,3-bis(trimethylsilyl)alk-3-en-1-ynes 2, which underwent a desilylation reaction to afford ( Z)-3-(trimethylsilyl)alk-3-en-1-ynes 3 in high yields. (1 E,3 Z)-1-Halo-3-(trimethylsilyl)-substituted 1,3-dienes 5 could be synthesised stereoselectively via hydrozirconation of ( Z)-3-(trimethylsilyl)alk-3-en-1-ynes 3, followed by trapping with iodine or N-bromosuccinimide.
Moniline, A New Alkaloid from Dendrobium moniliforme
Authors: Liu Wen-Hong , Hua Yun-Fen , Zhan Zha-Jun
Published: December 2009

A new alkaloid, moniline (1), and a known alkaloid 6-hydroxynobiline (2) were isolated from the stems and leaves of Dendrobium moniliforme. The structure of 1 was established by spectroscopic methods, especially 2D NMR techniques.
Rate and Product Studies in the Solvolyses of Two Arenesulfonic Anhydrides
Authors: Kevill Dennis N. , Ryu Zoon Ha
Published: December 2009

The specific rates of solvolysis of benzenesulfonic anhydride (1) and p-toluenesulfonic anhydride (2) have been measured conductometrically at −10°C in 34 solvents for 1 and 33 solvents for 2. Studies at higher temperatures have allowed extrapolated values in additional solvents to be calculated. All of the values, for 35 solvents for 1 and for 37 solvents for 2, have been used in an extended Grunwald–Winstein equation treatment using NT and YOTs values. Activation parameters in several solvents and kinetic solvent isotope effects (MeOH/MeOD) have been determined for both substrates. Product selectivity values ( S) have been determined for binary mixtures of water with ethanol, methanol, or 2, 2, 2-trifluoroethanol. The results from the kinetic and product studies are compared to those previously reported for methanesulfonic anhydride (3). An SN2 mechanism is proposed for the solvolytic displacement reactions of the three substrates in all of the solvents used in the investigation.
Oxidative deprotection of tetrahydropyranyl and trimethylsilyl ethers in water using 1,4-dichloro-1,4-diazoniabicyclo[2,2,2]octane bis-chloride under neutral conditions
Authors: Tajbakhsh Mahmood , Habibzadeh Setareh
Published: December 2009

A facile oxidative deprotection of trimethylsilyl and tetrahydropyranyl ethers in water using 1,4-dichloro-1,4-diazoniabicyclo[2,2,2]octane bis-chloride as a new efficient reagent under neutral conditions is described. This methodology is ecofriendly and environmentally benign since it uses water as a solvent. In all reactions DABCO was regenerated, rechlorinated and reused several times.
Solventless Wittig Olefination with Fluorinated Benzaldehydes
Authors: Thiemann Thies
Published: December 2009

Fluorinated benzaldehydes undergo solventless Wittig olefination with stabilised phosphoranes. Even with less reactive, stabilised phosphoranes, such as acetylmethylidenetriphenylphosphorane, the reactions have been found to be exothermic.
Synthesis and Variable Temperature 1H and 31P NMR Study of Phosphorus Ylides derived from reaction of NH-acids, triarylphosphine and acetylenic esters
Authors: Sabounchei Seyyed Javad , Nemattalab Hassan
Published: December 2009

A one-step synthesis of sterically congested phosphorus ylides in moderate to good yields by the reaction of dialkyl acetylenedicarboxylates, NH-acids and triarylphosphines are reported. Characterisation of the obtained compounds was performed by IR, 1H, 31P, 13C NMR, elemental analysis and mass spectroscopy. NMR spectra showed that some of these compounds (in CDCl3 as solvent) contained two rotamers with unequal populations that equilibrate rapidly at higher temperatures.
Synthesis of New Quinazoline-2,4(1H,3H)-dione non-nucleoside Analogues of the reverse transcriptase inhibitor TNK-651
Authors: El-Brollosy Nasser R.
Published: December 2009

The synthesis is described of a series of new non-nucleoside analogues of the reverse transcriptase inhibitor TNK-651 from quinazoline-2,4(1 H,3 H)-diones. Compounds 2a–c were silylated and treated with benzyl chloromethyl ether in the presence of CsI to give 1-benzyloxymethylquinazoline derivatives 3a–c. Treatment of the silylated quinazolinediones 2a–c with the appropriate acetals 5a–e in the presence of TMS triflate afforded the corresponding TNK-651 analogues 6–10.
A Study on the Electronic Effect of para-substituents in the Aryloxy Ring of the Hydrazone Ligands on the Vanadium Centre in the mixed-ligand [VIVO(ONO)(NN)] families
Authors: Ghosh Tapas , Mondal Bipul
Published: December 2009

The hyperfine coupling constant (Aıı) and the redox potential (E½) values of vanadium(IV) in its mixed-ligand hydrazone complexes [VIVO(L)(bipy)], 1–4 and [VIVO(L)(phen)], 5–8, [which have been synthesised from the reaction of VIVO(acac)2 with the hydrazone ligand H2L in the presence of equimolar amount of 2,2′-bipyridine (bipy) or 1,10-phenanthroline (phen) in methanol], exhibit a linear relationship with the Hammett constant (σ) of the para-substituents in the aryloxy ring of the hydrazone ligands.
Regio- and diastereo-selective formation of Isoxazoline Derivatives by Lewis acid Mediated 1,3-dipolar Cycloaddition Reactions of Nitrile Oxide
Authors: Hayashi Saori , Mori Akira , Nishina Masatoshi , Sumimoto Masanori , Hori Kenzi , Yamamoto Hidetoshi
Published: December 2009

In the presence of magnesium perchlorate, 1,3-dipolar cycloaddition reactions of nitrile oxides to crotonamide bearing 4-benzyl-5,5-dimethyl-1,3-oxazolidin-2-one as the chiral auxiliary proceeded with a regio- and diastereo-selective manner to afford the corresponding chiral 2-isoxazoline. The mechanisms underlying the diastereoface selection in the cycloaddition reaction were investigated using the B3LYP/6-31G* level of theory.
A One-Pot, Stereoselective Synthesis of (Z)-1,2-disubstituted Vinyl Sulfides by Sequential Hydrostannylation and Stille reaction of Acetylenic Sulfides with Tributyltin Hydride and then with aryl iodides
Authors: Hao Wenyan , Wang Dong , Cai Mingzhong
Published: December 2009

( Z)-1,2-Disubstituted vinyl sulfides can be stereoselectively synthesised in one pot under mild conditions, in good yields, by the palladium-catalysed hydrostannylation of acetylenic sulfides, followed by Stille coupling with aryl iodides.
Unprecedented Photoinduced Insertion Reactions of N-methyl-1,2-naphthalenedicarboximide with Phenylacetylene
Authors: Liu Qingjian
Published: December 2009

Irradiation of N-methyl-1,2-naphthalendicarboximide 1 together with phenylacetylene in benzene afforded unprecedented reductive insertion products dihydronaphthazepinediones 2a and 2b, which were characterised by NMR spectroscopy (1H, 13C), IR spectroscopy, MS, elemental analysis and assignments confirmed by X-ray crystallographic analysis.
Synthesis and Complexation Behaviour of Tetrakis[(N,N-diethylamino-carbonyl)methoxy]tetrahomodioxacalix[4]arene
Authors: Takimoto Masashi , Aramaki Takashi , Xi Zeng , Yamato Takehiko
Published: December 2009

O-Alkylation of the flexible tetrahomodioxacalix[4]arene 1 with N,N-diethylchloroacetamide in the presence of NaH, K2CO3 or Cs2CO3 gave only one pure stereoisomer, 1,4- alternate-2, while other possible isomers were not observed.
A Synthesis of 1-aryl-3,5-dioxo-tetrahydro-1H-pyrazols from reaction of Alkyl Isocyanides, Isopropylidene Meldrum's Acid and Arylhydrazines
Authors: Yavari Issa , Sabbaghan Maryam , Ghazanfarpour-Darjani Majid , Hossaini Zinatossadat
Published: December 2009

The reaction between alkyl isocyanides and isopropylidene Meldrum's acid in the presence of arylhydrazines leads to functionalised 1-aryl-3,5-dioxo-tetrahydro-1 H-pyrazols in good yields.
Ph3P promoted one-pot synthesis of dialkyl 2-(2-oxopyridin-1(2H)-yl)but-2-enedioates from a reaction of 2-hydroxypyridine and dialkyl acetylenedicarboxylates
Authors: Yavari Issa , Alborzi Ali R. , Mohtat Bita
Published: December 2009

2-Hydroxypyridine undergoes a smooth reaction with dialkyl acetylenedicarboxylates in the presence of triphenylphosphine (15 mol%) to produce the E/Z isomers of dialkyl 2-(2-oxopyridin-1(2 H)-yl)but-2-enedioates in high yields.
Correlation between Redox Properties and Component of Multicomponent Heteropolysilicates with the Same Structure
Authors: Hua Chunyan , Li Jiang , Ding Hanmin , He Pingang , Shan Yongkui
Published: December 2009

A series of the multicomponent heteropolysilicates with the same structure has been synthesised by a controllable method. Studies on the correlation between the redox properties and composition of the polyoxometalates indicate that the character of the addenda ion has the highest influence on the oxidising ability of the heteropolyanions for a given structure, and by comparison, the effects of the number of the addenda ions and the charge of the whole heteropolyanions were not completely prominent in mixed-addenda tungstomolybdosilicate heteropolyanions. For transition metal-substituted heteropolyanions, however, the effect of the number of the addenda ions is an important factor and stronger than that of the character of the addenda ion (transition metal ion) in some cases. On the other hand, incorporation of a transition metal ion can lead to a decrease of the reversibility of redox for heteropolyanions.
One-pot Synthesis of the derivatives of 2-cyclopent-2-en-1-one by SOCl2/EtOH
Authors: Hu Zhiguo , Dong Zhibing
Published: December 2009

A simple and efficient method for the synthesis of derivatives of cyclopent-2-en-1-one is presented. Aromatic aldehydes reacted with aliphatic ketones in the presence of thionyl chloride in anhydrous ethanol to give seven derivatives of 2-cyclopenten-1-one in one step with reasonable yields. The structures of the products were established.
Asymmetric-Catalysed Preparation and Stereochemistry of (R,R)-,(S,R)-(6-Fluoro-2-Chromanyl)-1,2-Ethanediol
Authors: Yang Yun-Xu , Liu Shi-Xiang
Published: December 2009

(R,R)-,(S,R)-1-(6-fluoro-2-chromanyl)-1,2-ethanediol 1a/1b were prepared by hydrolytic kinetic resolution (HKR) of terminal racemic epoxides using (R,R)-SalenCo(OAc) as a catalyst. Their configurations were established by comparison with two authentic samples by HPLC.
Reaction of 4-Chloro-3,5-Dinitrobenzotrifluoride with Aniline Derivatives. Substituent Effects
Authors: Al-Howsaway Hamida O.M. , Fathalla Magda F. , El-Bardan Ali A. , Hamed Ezzat A.
Published: December 2009

N-(2,6-Dinitro-4-trifluoromethylphenyl)aniline derivatives were prepared by anilino-dechlorination of 4-chloro-3, 5-dinitrobenzotrifluoride. IR, UV and 1H NMR studies suggested an intramolecular hydrogen bond between the amino hydrogen and one o-nitro group. An addition-elimination mechanism was suggested based on the second-order kinetics and the dependence of rates on the nature and the position of the substituent in the aniline ring, as well as the high negative values of ρ(-3.14, −3.16, −3.01). Such values indicate a positive charge on the aniline nitrogen in the transition state and that the rate is affected by the polar effect of the substituent. The β value (0.85 at 30°C) indicates an appreciable degree of bond formation in the transition state.
Studies with 2-Arylhydrazononitriles: Further Investigations on the Utility of 2-Arylhydrazononitriles as Precursors to 1,2,3-Triazole Amines
Authors: Al-Mousawi Saleh Mohammed , Moustafa Moustafa Sherief , Elnagdi Mohamed Hilmy
Published: December 2009

3-Oxo-2-arylhydrazonobutanenitriles react with hydroxylamine hydrochloride in ethanolic sodium acetate to yield either amidoximes or isoxazolamines depending on the nature of the substituent. The amidoximes cyclise in refluxing DMF containing piperidine to form 2-aryl-1,2,3-triazol-5-amines. The isoxazolamines rearranged into 1,2,3-triazolamines on refluxing in DMF. Amidoxime 2c cyclised in acetic anhydride to give 2-arylhydrazono-1,2,4-oxadiazole 9c, which rearranged to acetylamino-1,2,3-triazole 8c. The prepared acetyl-1,2,3-triazolamines 8b,c were utilised as precursors to triazolopyridines and pyrazolyltriazoles.
Catalytic Activity of [Rh(CO)2(bBzlH2py)]Cl.1.5H2O and [CoCl(bBzlH2py)2] Cl.2H2O
Authors: Alexander Stanislaus , Gayathri Virupaiah , Nanjegowda Nadur Muddanna
Published: December 2009

The complex [Rh(CO)2(bBzlH2py)]Cl.1.5H2O [bBzlH2py = 2,6-bis(benzimidazolyl)pyridine] reversibly binds CO and in alcoholic solvents loses CO to form yellow [RhCl(bBzlH2py)(OH2)].H2O. When NO or O2 gas was passed through a 2-methoxy ethanolic solution of [Rh(CO)2(bBzlH2py)]Cl, formation of CO2 was observed. Hence the possible catalytic activity of the complex towards the reactions NO + CO, CO + O2, and NO + O2 was studied and the NO + CO system is quite promising. The complexes [Rh(CO)2(bBzlH2py)]Cl.1.5H2O and [CoCl(bBzlH2py)2]Cl.2H2O were tested for their possible catalytic activity towards oxidation of alcohols using O2 and H2O2/O2 as oxidants. These complexes in the presence of H2O2 at refluxing temperature convert alcohols to aldehydes/ketones/acids.
Synthesis of Functionalised Titanocene Complexes
Authors: Zhang Ming , Zhang Ai-Qin , Chen Huan-Huan , Chen Jun , Chen Hai-Yan
Published: December 2009

Two functionalised titanocene complexes were synthesised from fulvene as starting material.
Etherification of (E)-1,3-Diaryl- and (E)-1,3-Diheteroaryl- Prop-2-en-1-ols with Primary and Secondary Alcohols over Platinum on Carbon
Authors: Thiemann Thies
Published: December 2009

In the presence of platinum on carbon (Pt/C), (E)-1,3-diaryl- and (E)-1,3-diheteroaryl- prop-2-en-1-ols react with primary and secondary alcohols to give (E)-1,3-diaryl- and (E)-1,3-diheteroaryl- prop-2-enyl ethers.
Direct Reaction of Silica Gel with Butyllithium
Authors: Guthrie Robert D.
Published: December 2009

Silica gel with a variety of surface areas is found to react directly (no SOCl2 treatment required) with butyllithium to give a product with butyl groups attached. The extent of butyl group incorporation depends on available silica surface. With dehydrated 230–400 mesh silica gel, 7.4 mmoles of BuLi per g in pentane added in hexane gave silica with 2.5 mmoles of butyl groups per g provided that the silica gel was washed three times with cold water. It was found that water washing removes some unbutylated silicate increasing the apparent butyl group incorporation. The butyl-modified silica gel showed no chromatographic retention of 3-aminoquinoline in 50:50 hexane: dichloromethane or of thymol in hexane in contrast to unmodified silica gel which is known to strongly retain polar compounds, particularly basic ones. This contrast is demonstrated.
Synthesis and Structure Determination of 2,3-Diphenyl-2H-1,4-Benzoxazin-2-ol
Authors: Marjani Katayoun , Asgarian Jafar , Mousavi Mohsen
Published: December 2009

A stable hemiacetal, 2,3-diphenyl-2H-1,4-benzoxazin-2-ol, was isolated as the main product from the reaction of benzil and o-aminophenol in THF. The structure of the product is confirmed by elemental analysis, common spectroscopic methods, and X-ray crystallographic analysis.
Synthesis of 3-Aryl-3,4-Dihydroquinazolin-2(1H)-Ones with the Aid of Low-Valent Titanium Reagent (TiCl4-Sm)
Authors: Shi Daqing , Dou Guolan , Li Zheng-Yi
Published: December 2009

A short and facile synthesis of a series of 3-aryl-3,4-dihydroquinazolin-2(1H)-ones was accomplished in good yields via the novel reductive cyclisation of 2-nitrobenzylamines with bis(trichloromethyl)carbonate (triphosgene) promoted by TiCl4/Sm system. The structures of the products were characterised by IR, 1H NMR and elemental analysis and the structure of 3a was confirmed by X-ray diffraction analysis.
New 2,3-Disubstituted Quinazolin-4(3H)-Ones from 2-Undecyl-3,1-Benzoxazin-4-One
Authors: Mahmoud Mahmoud R. , El-Bordany Eman A.A. , Hassan Naglaa F. , El-Azm Fatma S.M. Abu
Published: December 2009

2-undecyl-4H-3,1-benzoxazin-4-one (2) was prepared and reacted with primary and secondary amines affording compounds 3–7, while with hydrazine hydrate it gave the quinazolinone derivative 8. The reaction of 8 with 3,4,5-trimethoxybenzaldehyde followed by thioglycollic acid yielded 9 and 10, respectively. Acylation of 8 using cinnamoyl chloride gave 11. Furthermore, treatment of 2 with hydrazine derivatives provided 12 and 13. Fusion of 2 with ammonium acetate gave the quinazolinone derivative 14 which upon treatment with ethyl chloroacetate yielded the ester 15. The hydrazide 17 was obtained from hydrazinolysis of the ester 15.
A Facile Synthesis and Heteroannulation of Thiazolopyrimidine and Related Heterocyclic Systems
Authors: Aly Aly A.
Published: December 2009

Reaction of pyrimidinylacetic acid 2 with different electrophilic and nucleophilic reagents gave annulated pyrimidine derivatives 3–11, respectively. Compound 3 ([7-(dibenzothien-2-yl)-5-phenyl-2,3-dihydro-5H-thiazolo[3,2-a]-pyrimidin-6-yl]acetic acid) was transformed to pyrimidinylacetyl azide 12, which upon heterocyclisation with active methylene compounds, acidic and basic reagents furnished functionally substituted heteroaromatic compounds 13–21, respectively. The structures of the synthesised derivatives were elucidated by elemental and spectral analyses.
One-pot Synthesis of Functionalised Keteneimines by three Component reaction of Isocyanides, Dialkyl acetylenedicarboxylates, and 4-phenylaminocoumarin
Authors: Anary-Abbasinejad Mohammad , Anaraky-Ardakani Hossain , Rastegari Forough , Hassanabadi Alireza
Published: December 2009

The reactive intermediate generated by the reaction of alkyl isocyanides and dialkyl acetylenedicarboxylates was trapped by 4-phenylaminocoumarin to produce dialkyl 2-cyclohexylamino-5-oxo-4 H,5 H-pyrano[3,2- c]chromene-3,4-dicarboxylates in good yields.
Spectroscopic and Theoretical Studies on Symmetric Aryl Azines
Authors: Karthikeyan Balakrishnan , Jayabharathi Jayaraman , Thanikachalam Venugopal
Published: December 2009

Azines, which closely resemble azobenzenes, have important applications in the field of nonlinear optics. NMR and IR spectroscopic study of some symmetric aryl azines has been undertaken with the aid of ab initio theoretical calculations. All data indicated that the structure of azine and substituted azines is the symmetric trans form.
Perfluorinated Sulfonic acid Resin (Nafion-H) catalysed Ritter reaction of Benzyl Alcohols
Authors: Yamato Takehiko , Hu Jian-yong , Shinoda Naoki
Published: December 2009

Perfluorinated sulfonic acid resin (Nafion-H) catalyst found to be effective in promoting the Ritter reaction of benzyl alcohols with nitriles such as acetonitrile, acrylonitrile and benzonitrile to give the corresponding N-benzylamides.
Medium-size Cyclophanes, 77.1 Synthesis and addition of Bromine to syn-[2.n]meta-cyclophan-1-enes
Authors: Saisyo Tatsunori , Shiino Mikiko , Hu Jian-yong , Yamato Takehiko
Published: December 2009

McMurry cyclisation of 1, n-bis(3-formyl-2-methoxyphenyl)alkanes afforded syn-dimethoxy[2. n]metacyclophan-1-enes, in which cis-addition of bromine to the bridged double bond in CH2Cl2 was observed.
New Synthesis of 1,3-diaryl-4-nitro-1-butanones by Microwave-Promoted Michael Addition of Nitromethane to Chalcones without Solvent
Authors: Li Shuangshuang , Xie Zengyang , Bian Xiaoqin , Wang Cunde
Published: December 2009

The Michael addition of nitromethane to chalcones promoted by microwave irradiation without solvent afforded 1,3-diaryl-4-nitro-1-butanones in good yield. The products were characterised by IR, 1H NMR and elemental analysis.
Three-Component reaction between 2-naphthol, Aromatic Aldehydes and Acetonitrile in the Presence of Chlorosulfonic Acid Yields 1-(Acetylamino (Aryl)Methyl)-2-Naphthols
Authors: Anary-Abbasinejad Mohammad , Hassanabadi Alireza , Kamali-Gharamaleki Maryam , Saidipoor Azimeh , Anaraki-Ardakani Hossein
Published: December 2009

The one-pot, three-component reaction between aryl aldehydes, 2-naphthol, and acetonitrile in the presence of chlorosulfonic acid affords 1-[acetylamino(aryl)methyl]-2-naphthols in excellent yields.
Synthesis and Structural Properties of Novel Calixarene Analogues having Schiff Base Units
Authors: Yamato Takehiko , Miyamoto Shinpei , Takimoto Masashi , Thuéry Pierre
Published: December 2009

Novel calixarene analogues having Schiff base units have been synthesised by condensation reaction of the bisaldehyde with o-phenylenediamines in the presence of boric acid. The present calixarene analogues form hydrogen bonds between imine nitrogen and phenol hydrogen with 1,2-alternate conformation, confirmed by X-ray crystallography.
Unusual product from the reaction of 2-diazo-1-[5-(4-methoxybenzoyl)-2,3-dihydropyrrolizin-1-yl]ethanone with rhodium (II) acetate
Authors: Cuevas-Yañez Erick , Hernández-Ortega Simón , Fuentes-Benites Aydeé , González-Romero Carlos , Cruz-Almanza Raymundo
Published: December 2009

The rhodium(II)-catalysed reaction of the diazoketone derived from 5-(4-methoxybenzoyl)-2,3-dihydropyrrolizin-1-carboxylic acid (anirolac) did not give the expected intramolecular cyclisation product but afforded the 2,3-dihydropyrrolizin-1-one only an elimination product. X-ray studies confirmed the structure.
[3,1]Oxazino[5′,4′:5,6]-, pyrido[3′,2′:5,6]-, pyrimidino[5′,4′:5,6]-, and pyrrolo[3′,2′:5,6]pyrano[3,2-c]chromene derivatives from 9-amino-7-(4-chlorophenyl)-6-oxo-6H,7H-pyrano[3,2-c]chromene-8-carbonitrile
Authors: Mahmoud Mahmoud R. , Madkour Hassan M.F. , El-Bordainy Eman A. , Soliman El-Said A.
Published: December 2009

Pyrido[3′,2′:5,6]-, [3,1]Oxazino[5′,4′:5,6]-, pyrimidino[5′,4′:5,6]-, and pyrrolo[3′,2′:5,6] pyrano[3,2- c]chromene derivatives were obtained via the reaction of 9-amino-7-(4-chlorophenyl)-6-oxo-6 H,7 H-pyrano[3,2- c]chromene-8-carbonitrile 1 with diethyl malonate, Schiff's base, acetic acid, phenyl isothiocyanate and chloroacetic acid, respectively. Alkylation, acylation and hydrazinolysis of 1 were also discussed. The IR, 1H NMR, 13C NMR and MS spectra of the synthesised compounds were discussed.
Synthesis of pyrido[2′,3′:4,5]thieno[2,3-d]pyrimidines through Friedländer reactions
Authors: Abdel-Mohsen Shawkat A. , Geies Ahmed A.
Published: December 2009

A variety of tri-, tetra- and penta–cyclic pyrido[2′,3′:4,5]thieno[2,3- d]pyrimidines have been synthesised from 5-amino-6-formyl-4-methyl-2-phenylthieno[2,3- d]pyrimidine by Friedländer condensation with aliphatic, alicyclic, and heterocyclic ketones and other active methylene compounds.
Zirconium Tetrachloride Catalysed Synthesis of Symmetric and Unsymmetric Ethers from Secondary Benzylic Alcohols
Authors: Das Biswanath , Krishnaiah Maddeboina , Veeranjaneyulu Boyapati , Srinivas Yallamalla , Rao Yerra Koteswara
Published: December 2009

Secondary benzylic alcohols are coupled in the presence of zirconium tetrachloride to afford the corresponding symmetrical ethers in good yields. Unsymmetric ethers are obtained with good selectivity by condensation of two different secondary benzylic alcohols under the action of the same catalyst.
Synthesis and Cytotoxicity of Analogues of the Marine Secondary Metabolite, 2-Deoxylapachol
Authors: Sunassee Suthananda N. , van Wyk Albert W.W. , Osoniyi Omolaja , Hendricks Denver T. , Davies-Coleman Michael T.
Published: December 2009

The syntheses of four 2-substituted 1,4 naphthoquinones, related to the marine natural product 2-deoxylapachol, are reported. All four synthetic compounds were cytotoxic to WHCO1 oesophageal cancer cells.
2-Acetyl-2,3,4,9-tetrahydro-1H-carbazol-1-one in the Synthesis of Heteroannulated Carbazoles
Authors: Martin Arputharaj Ebenezer , Prasad Karnam Jayarampillai Rajendra
Published: December 2009

The reaction of 2,3,4,9-tetrahydro-1 H-carbazol-1-ones with ethyl acetate yielded 2-acetyl-1-hydroxycarbazole and 2-acetyl-2,3,4,9-tetrahydro-1 H-carbazol-1-one. These were used to prepare isoxazolo- and pyrazolo-fused carbazoles. Mechanisms for the formation of the end products are proposed.
Synthesis and Characterisation of the Lithium, Sodium and Potassium Americium(β) Complexes of Hexaoxoperiodate: MI2[Am(OH)2H2IO6].xH2O
Authors: Qi Xinhua , Jia Xueqing , Yang Ying , Gao YaPing , Niu Li-e
Published: December 2009

Novel complexes of trivalent Americium with hexaoxoperiodate have been prepared for the first time from an aqueous caustic solution. Chemical analysis indicated that the composition of the complexes is MI2[Am(OH)2H2IO6]. xH2O (MI = alkali metal: x = 4, MI = Na, K; X = 11, MI = Li) and all the complexes have been characterised by X-ray powder diffraction, UV-Visible, IR, and Raman spectroscopic studies, and by thermal analysis.
Synthesis and Characterisation of Hg (II) and Ag (I) Complexes of 4-Fluorobenzoylmethylenetriphenylphosphorane and 4-chlorobenzoyl methylenetriphenylphosphorane, with Spectroscopic Studies
Authors: Karami Kazem
Published: December 2009

4-flourobenzyloxymethylenetriphenylphosphorane ylide [Ph3PCHCOC6H4F], (FBPPY), and 4-chlorobenzyloxymethylenetriphenylphosphorane ylide [Ph3PCHCOC6H4Cl],(CBPPY), have been synthesised. The reactions of the title ylides with HgX2 (X =Cl,I) in equimolar ratios using dry acetone as solvent, have yielded [{HgCl2(FBPPY)}2](1), [{HgI2(FBPPY)}2](2), [{HgCl2(CBPPY)}2](3) and [{HgI2 (CBPPY)}2](4) respectively. The reactions of the title ylides with AgNO3 in molar ratios (2:1) using dry acetone as solvent have yielded [Ag(FBPPY)2]NO3(5) and [Ag(CBPPY)2]NO3(6). The analytical data, IR and 1H and 31P NMR data of the products were obtained.
Synthesis of thieno[2,3-b][1,6]naphthyridines and pyrimido[4′,5′:4,5] thieno[2,3-b][1,6]naphthyridines
Authors: Abdel-Wadood Fatma K. , Abdel-Monem Maisa I. , Fahmy Atiat M. , Geies Ahmed A.
Published: December 2009

3-Cyano-6-methyl-5,6,7,8-tetrahydro[1,6]naphthyridine-2(1H)-thione (3a) and 3-cyano-6-methyl-4-(2′-thienyl)-5,6,7,8-tetrahydro[1,6]naphthyridine-2(1H)-thione (3b) were reacted with α-halo compounds to give the intermediates 4a–j which upon refluxing in ethanolic sodium ethoxide afforded the thieno[2,3-b][1,6]naphthyridine derivatives 5a–l. Further annellation of pyridine and pyrimidine rings to the remaining free bond of the fused thiophene ring was achieved, providing tetrahydro-pyrido[2′,3′:4,5]- and -pyrimido[4′,5′:4,5]-thieno[2,3-b][1,6]naphthyridines. Some of the synthesised compounds were screened against different strains of bacteria.
Stable phosphorus ylides and heterocyclic phosphonate esters derivatives synthesised from stereoselective reactions between triphenyl phosphite and activated acetylenic esters
Authors: Maghsoodlou Malek Taher , Habibi-Khorassani Sayyed Mostafa , Nassiri Mahmoud , Adhamdoust Sayyed Reza , Salehzadeh Jaber
Published: December 2009

One-pot synthesis of stable heterocyclic phosphorus ylides 4a–j is reported in fairly good yields by the reaction between dialkyl acetylenedicarboxylates and triphenyl phosphite in the presence of strong NH-acids such as 2-benzoxazolinone, 2-indolinone and 2-mercaptobenzoxazole in aqueous media as an environmentally friendly solvent. The hydrolysis of compounds 4a–f led to stable phosphonate ester derivatives 5h–l. The configuration of compounds 5h–l (2S*,3R*) was determined on the basis of coupling constant predicted from the Karplus equation.
Cycloaddition of benzo[b]thiophene-S,S-dioxide – a route to substituted dibenzothiophenes and dibenzothiophene S,S-dioxides
Authors: Iniesta Jesus , Matsumoto Taisuke , Thiemann Thies
Published: December 2009

Benzo[b]thiophene S,S-dioxide can be transformed by cycloaddition with tetraarylthiophene S-oxides to tetraaryldibenzothiophene S,S-dioxides. An analogous cycloaddition of benzo[b]thiophene S,S-dioxide, albeit at higher temperatures, leads directly to tetraaryldibenzothiophenes.
Oxadiazole, oxadiazine, oxadiazepine, pyrazole and tetrazole derivatives from substituted carbohydrazides
Authors: Hassan Alaa A. , Ibrahim Yusria R. , Shawky Ahmed M.
Published: December 2009

The condensation of substituted carbohydrazides 1a–e with a series of electron-poor compounds such as dimethyl but-2-ynediolate (2), 1,4-diphenylbut-2-yne-1,4-dione (3), 1,4-diphenylbut-2-ene-1,4-dione (4), and diethyl diazene-1,2-dicarboxylate (5) gave the derivatives of 1,3,4-oxadiazepine, 1,3,4-oxadiazinylacetate, (1,3,4-oxadiazolylidene) ethanone, dibenzoylpyrazole and tetrazolecarboxylate. The reaction mechanisms described the products formation are discussed.
Facile One-Pot synthesis of Some New 2-amino-4H-pyran Derivatives
Authors: Zonouzi Afsaneh , Rahmani Hossein , Kazemi Davoud , Izakian Zakieh
Published: December 2009

The one-pot reaction of alkylisocyanides 1 and acetylenic esters 2 in the presence of 1, 3-diketones 3 provides an efficient access to 2-amino-4 H-pyrans 4a–l. Ketenimines 5 were detected in the early stage of reaction as intermediates. The products 4a–l are stabilised by an intra molecular N-H…O hydrogen bonding.
Three-Component Synthesis of Fluorinated Pyrimidine Carbonitrile Derivatives under Thermal Aqueous Conditions
Authors: Sheibani Hassan , Saidi Kazem , Saljooghi Arman S.
Published: December 2009

A series of new fluorine containing 4-amino-pyrimidine-5-carbonitrile derivatives has been synthesised from the three-component reaction of malononitrile, fluorinated aldehydes or ketone and N-unsubstituted amidines. The reaction occurs in water at reflux and is microwave assisted. This method provides a new route to produce fluorinated pyrimidine derivatives in good to excellent yields.
Phototransformation of Some N-(2-hydroxy-1,3-dioxo-2,3-dihydro-1H-inden-2-yl)aryl/heterylamides
Authors: Kapoor Mona , Dhawan Som N. , Mor Satbir , Gupta Satish C.
Published: December 2009

Photoreorganisation of few N-(2-hydroxy-1,3-dioxo-2,3-dihydro-1 H-inden-2-yl)aryl/heterylamides 1 to N-benzoyl-3-oxo-1,3-dihydro-2-benzofuran-1-carboxamides 2 is described
A New Eremophilane Sesquiterpene from Senecio Nemorensis
Authors: Meng Fanjun , Xie Weidong , Row Kyungho
Published: December 2009

A new eremophilane sesquiterpene was isolated from the MeOH extract of the aerial parts of Senecio nemorensis. Its structure was established as 11-hydroxy-1β-methoxyl-8-oxoeremophila-6,9-dien-12-oic methyl ester by extensive application of spectroscopic methods, including IR, EI-MS, HR-ESI-MS, 1D and 2D NMR spectroscopy.
Synthesis and X-ray Crystallographic Analysis of a bis(arylmethylidene) Pyranone Structure
Authors: Abaee M. Saeed , Mojtahedi Mohammad M. , Sharifi Roholah , Zahedi Mohammad M. , Mesbah A. Wahid , Massa Werner
Published: December 2009

The exocyclic olefinic bonds and their E-E configuration in a bis(arylmethylidene)pyranone system are confirmed for the first time by X-ray crystallography of the 3,5-dibenzylidene-tetrahydropyran-4-one derivative.
K2S2O8/MoO3: An Oxidation Reagent for benzylic alcohols and trimethylsilyl and tetrahydropyranyl ethers
Authors: Shirini F. , Yazdanbakhsh M.R. , Pop-Kiadeh M. Mahdavi , Abedini M.
Published: December 2009

The oxidation of benzylic alcohols and trimethylsilyl (TMS) and tetrahydropyranyl (THP) ethers to their corresponding carbonyl compounds with K2S2O8 is efficiently promoted by the presence of MoO3.
Synthesis of Thiadiazine, Imidazothiadiazole, Diazospiroundecatetraene and Spirothiadiazolopyrimidinocyclohexadiene Derivatives from 2,5-Dithiobiureas
Authors: Hassan Alaa A. , Aly Ashraf A. , El-Sheref Essmat M.
Published: December 2009

Ethenetetracarbonitrile (2, in tetrahydrofuran solution), diethyl (E)-2,3-dicyanobutenedioate (10, in tetrahydrofuran solution), and 7,7′,8,8′-tetracyanoquinodimethane (16, in pyridine solution) act on 1-substituted-2,5-dithiobiureas 1a–c, forming the derivatives of imidazothiadiazole 5a–c, thiadiazine 11a–c and 12a–c, spiro(thiadiazolopyrimidinocyclohexadiene)malononitrile 17a–c and diazospiroundecatetraene 18a–c. Rationales for these conversions involving the nucleophilic addition on diycanomethylene carbon atom are presented.
The Regio-and Stereo-Chemistry of 1,3-Dipolar Cycloaddition of a Chiral Methylenenitrone to 1,2-Disubstituted Alkenes
Authors: Ali Shaikh A. , Iman Muhammad Z.N.
Published: December 2009

A study of regio- and stereo-selectivity in the cycloaddition reactions of a series of symmetrical and unsymmetrical 1,2-disubstituted alkenes to the chiral, internally H-bonded N-(2-hydroxy-1-phenyl)methylenenitrone, has been carried out. The regioselectivity observed in the addition reactions is explained in terms of frontier orbital interactions. The alkenes having a hydroxymethyl substituent at the allylic position are found to undergo regio- as well as highly stereo-selective cycloaddition reactions in the presence of anhydrous magnesium bromide.
Synthesis of Some New Pyrazolo[1,5-a]Pyrimidines
Authors: Ahmed Sayed A. , Abdelhamid Abdou O. , El-Ghandour Ahmed H. H. , Mohamed Mahmoud A. , Mohamed Basant M.
Published: December 2009

Pyrazolo[1,5-a]pyrimidines were synthesised from the the reaction of β-diketone, β-keto ester, 1,2-disubstituted acrylonitrile or sodium (3-oxocycloalkylidene) methenolate. Elemental analysis, spectral data and alternative synthesis route elucidated structures of the newly synthesised compounds.
7-Methyl-9-Oxo-Dec-7-Eneoic Acid from the Red Sea Sponge Ircinia Sp
Authors: Tatli I. Irem , Kong F. , Feng Xidong , Carter Guy , Rao Karumanchi V. , Hamann Mark T.
Published: December 2009

An NMR and ultra-high resolution mass investigation of secondary metabolites from a Red Sea sponge Ircinia sp. led to the isolation and characterisation of a new ketone. The structure has been assigned on the basis of detailed spectroscopic analysis (1H, 13C, DEPT, COSY, HMQC and HMBC NMR spectra) as 7-methyl-9-oxo-dec-7-eneoic acid (1). Ultra-high resolution FTMS was utilised to facilitate the formulation and structure assignment because there was a broad and undetectable carbon signal in the NMR spectra.
Preparation of N-alkyl-substituted 3,5-dinitroanilines by amination of 1,3,5-trinitrobenzene
Authors: Qian Chao , Liu Jinqiang , Chen Xinzhi
Published: December 2009

Highly efficient amination of 1,3,5-trinitrobenzene by a number of simple aliphatic amines to form the corresponding N-alkyl-substituted 3,5-dinitroanilines has been achieved.
One-pot synthesis of novel 1,2,3,4,5a,7,8,8b-octaaza-acenaphthylenes
Authors: Shawali Ahmad S. , Mosselhi Mosselhi A. N. , Abdallah Magda A. , Elewa Mahmoud S.
Published: December 2009

Reaction of 4-amino-4H-1,2,4-triazole-3,5-dithiol 1a with hydrazonoyl halides 2 in ethanol in the presence of sodium ethoxide under reflux led to the formation of the title compounds 5. The latter products can also obtained by reaction of 4-amino-3,5-di(methylthio)-4H-1,2,4-triazole 1b with hydrazonoyl halides 2 in ethanol in the presence of sodium ethoxide by stirring over night at room temperature. The structures of the products were evidenced by spectral, elemental as well as X-ray diffraction analyses. The mechanism of the studied reactions was also discussed.
Novel isocoumarin and isoquinoline derivatives
Authors: Mahmoud Mahmoud R. , El-Shahawi Manal M. , Farahat Samira E.
Published: December 2009

A number of novel isoquinoline-1,3-dione derivatives have been synthesised using the readily obtainable anhydride formed from the Stobbe-type condensation of diethyl homophthalate with p-anisaldehyde. Primary amines form amides at the C-1 carbonyl group; recyclisation gives 4-(4-methoxybenzylidene)isoquinoline-1,3-diones.
A concise synthesis of (R)-Bgugaine, a pyrrolidine alkaloid from arisarum vulgare
Authors: Majik Mahesh S. , Parameswaran P.S. , Tilve Santosh G.
Published: December 2009

A new short method for the preparation of (R)-Bgugaine (1) has been described using Wittig condensation of a non-stabilised ylide with N-carboethoxy prolinal followed by reduction of double bond and conversion of N-carboethoxy group to N-methyl.
The X-ray crystal structure of 2,4-bis(4-methoxyphenoxy) pyrimidine
Authors: De Amitabha , Biswas Goutam , Muhonen Heikki
Published: December 2009

The X-ray crystal structure of 2,4-bis(4-methoxyphenoxy)pyrimidine, C18H16N2O4 was stabilised by the hydrogen bonding and van der Waal forces. The C-N bond in the pyrimidine moiety is shortened indicating of immonium character and good hydrogen bond donor potential. Both the phenyl rings are nearly perpendicular to the pyrimidine rings. The dihedral angles between the phenyl rings and the pyrimidine ring are 85.6(1) and 87.2(1)°. In the crystal packing, the pyrimidine rings stack with the pyrimidine rings and phenyl rings stack with the phenyl rings. The weak C-H…O interactions and π–π stacking interactions generate chains of molecules that are linked into sheets about the inversion centres.
Design, synthesis and biological activities of novel 1,2,3-thiadiazole derivatives containing oxime ether
Authors: Dong Wei-li , Yao Hong-wei , Li Zheng-ming , Zhao Wei-guang
Published: December 2009

A series of novel 2-methoxyimino-1,2,3-thiadiazole-5-acetamide derivatives were synthesised. Their structures were identified by means of elemental analysis, IR, 1H NMR and MS spectra. The preliminary biological activity tests showed that some of the compounds showed some fungicidal activity.
Photochromism and Crystal Structure of 3,3′-dimethyl-3,3′-dihydroxy-5, 5′-dimethyl-2,2′-bi-1H-indanylidene-1,1′-dione
Authors: Li Xu
Published: December 2009

A novel photochromic compound, 3,3′- dimethyl-3,3′-dihydroxy-5,5′-dimethyl -2,2′-bi-1H-indanylidene-1,1′-dione (I), was synthesised and its structure was determined by X-ray crystallography. The compound exhibited reversible photochromism, and a stable organic radical was generated which was detected by electron spin resonance spectroscopy.
Synthesis and optical properties of novel compounds containing carbazole and 1, 8-naphthalimide groups
Authors: Feng Guo-Liang , Ji Shun-Jun , Geng Li-Jun , Bian Bing , Liu Yu
Published: December 2009

A series of novel carbazole-naphthalimide compounds with moieties capable of carrier-balance and electroluminescence were synthesised and characterised, and theirs luminescent properties had been studied.
An Efficient Method for the Ring Opening of Epoxides with Aromatic Amines by Sb(III) Chloride under Microwave Irradiation
Authors: Ghazanfari Dadkhoda , Hashemi Mohammed M. , Mottaghi Mohammad Mehdi , Foroughi Mohammad Mehdi
Published: December 2009

SbCl3 supported on montmorillonite K-10 is an efficient catalyst for the ring opening of epoxides with aromatic amines under solvent-free conditions and microwave irradiation to give the corresponding β-amino alcohols in high yields with high regioselectivity
Bromination of Alkenes and Alkynes with (Bromodimethyl)Sulfonium Bromide
Authors: Das Biswanath , Srinivas Yallamalla , Sudhakar Chittaluri , Ravikanth Bommena
Published: December 2009

Alkenes and alkynes were brominated efficiently in high yields with (bromodimethyl)sulfonium bromide in acetonitrile at room temperature. Alkenes produced the corresponding trans-dibromo compounds while alkynes (except phenylacetylene) afforded both the trans-dibromo products (major) and the tetrabromo derivatives (minor). However, phenylacetylene furnished solely the tetrabromo compound.
A Simple Synthesis of Enaminones from Reaction between Isocyanides and Cyclic 1,3-dicarbonyl Compounds
Authors: Maghsoodlou Malek Taher , Hazeri Nourallah , Habibi-Khorassani Sayyed Mostafa , Solimani Vahideh , Marandi Ghasem , Razmjoo Zahra
Published: December 2009

Polarised olfinic systems are synthesised from the reaction between alkyl or aryl isocyanides and cyclic 1, 3-dicarbonyl compounds such as thiobarbituric acid, 5,5-dimethylcyclohexane-1,3-dione and cyclopentane-1,3-dione in good yield.
Fifty Years of the Synthesis of Labelled Mevalonic Acid
Authors: Hanson James R.
Published: December 2009

This article reviews developments in the synthesis of isotopically-labelled samples of mevalonic acid for use in studies of terpenoid and steroid biosynthesis.
Synthesis of Novel Amide-Linked Dimers of Lithocholic Acid
Authors: Joachimiak Roman , Piasecka Monika , Paryzek Zdzisław
Published: December 2009

An efficient synthesis of lithocholic amides and amide-linked dimers under mild conditions is described. New o-, m- and p-phenylenediamine-derived dimers of lithocholic acid were synthesised by the activation of the carboxyl group of the bile acid as a mixed anhydride resulting from the reaction of the acid with ethyl chloroformate. The reduction of lithocholic amides afforded the corresponding 24-amino-5β-cholane derivatives. All compounds were characterised by IR, 1H and 13C NMR and mass spectra.
Synthesis and antimicrobial screening of N-[coumarin-6-yl-amino] thiazolidinone and its derivatives
Authors: Mulwad Vinata V. , Mir Abid Ali
Published: December 2009

6-(2-Chloroacetyl)-aminocoumarins 2a-c were prepared by reacting the 6-aminocoumarins 1a-c and chloroacetylchloride in dry benzene. Compound 2a-c on treatment with thiourea yields 6-(2′-amino-1′,3′-thiazol-4′-yl)aminocoumarins 3a-c. Compounds 3a-c were treated with aromatic aldehydes, resulted in the formation of 6-(arylidenimino-1′-3′-thiazole-4′-yl)aminocoumarin 4a-f. The arylidenoiminos 4a-f on cyclisation with chloroacetylchloride/triethylamine and thioglycollic acid gave 6-[2′-(3”-chloro-2”-oxo-4”-phenyl-1”-azetidinyl)-1′,3′-thiazole-4′-yl]aminocoumarins 5a-f and 6-[2′-(2”-phenyl-4”-thiazolidinone-3”-yl)-1′, 3”-thiazole-4′-yl]aminocoumarin 6a-f respectively. Compounds 4a-f were also treated with aniline and sodium nitrite in the presence of conc. HCl to yield 6-[2′-(1”-phenyl-3”-phenylformazane-4”-yl)-1′,3′-thiazole-4′-yl]aminocoumarins 7a-f. The structure of these compounds have been established on the basis of their analytical and spectroscopic data. All the above compounds were screened for their antimicrobial activity. Some were found to show significant antimicrobial activity.
Synthesis of Indolones and Quinolones by Reductive Cyclisation of o-nitroaryl Acids using Zinc Dust and Ammonium Formate
Authors: Dinesh Bhima Reddy , Baba A. Ramesha , Sankar K. Udaya , Gowda D. Channe
Published: December 2009

A novel protocol for the synthesis of indolone and quinolone derivatives from o-nitroaryl acids was developed using Zn and HCO2NH4 under supercritical fluid carbon dioxide (scCO2) medium. The process involves the reduction of the nitro group to an amino group followed by in situ cyclisation.
Structural Analyses of tetrathiadodecahydro[3.3.3.3]paracyclophane Complexes with Copper(I) and Silver(I)
Authors: Yang Ya-Chen , Lin Shaw-Tao , Chen Wen-Shing
Published: December 2009

The preparation and X-ray structures of complexes of 2,11,20,29-tetrathia-4 e,5,6,7 e,8,9,22 e,23,24,25 e,26,27-dodecahydro[3.3.3.3]cyclophane (2) ( tTTDHPCP) with Cu(I), i.e. [Cu2I2( tTTDHPCP)]·thf 3, and with Ag(I), i.e. [Ag2 (tTTDHPCP)(CF3COO)2] 4, are reported. The sulfur atoms of compound 2 bind with metals to serve as the bridge in the polymeric structures, while anions interact with other metal atoms forming multi-dimensional structures. Complex 3 is a novel three-dimensional coordination polymer composed of Cu4 motifs, in which (CuI)2 forms a square planar unit to link the compound 2 molecules with a THF molecule situated outside the open cavities. In contrast, the Ag atom in complex 4 serves as a bridge for two compound 2 molecules, providing a two-dimensional channel framework. Unit cell data: complex 3, monoclinic system, space group P2(1)/n, a = 14.1935(19) Å, b = 13.7879(19) Å, c = 22.222(3) Å, β = 107.888(3)°, Z=4.; complex 4, triclinic system, space group P-1, a = 9.4736(7) Å, b = 12.0619(8) Å, c = 18.0914(10) Å, β = 80.1260(10)°, Z = 2.
Sulfamic Acid Catalysed One-Pot Three-Component Condensation for the Synthesis of 1,4-dihydropyrano[2,3-c]pyrazoles
Authors: Shinde Sandeep V. , Jadhav Wamanrao N. , Kondre Jeevan M. , Gampawar Sumit V. , Karade Nandkishor N.
Published: December 2009

A clean and simple synthesis of 6-amino-4-aryl-3-methyl-1-phenyl-1,4-dihydropyrano[2,3- c]pyrazole-5-carbonitriles was accomplished in good to excellent yields via the one-pot three component condensation of 3-methyl-1-phenyl-2-pyrazolin-5-one, an aromatic aldehyde, and malononitrile catalysed by sulfamic acid in ethanol.
Preparation of 5-oxo-5, 6, 7, 8-tetrahydro-4H-benzo-[b]-pyran Derivatives in Ionic Liquids
Authors: Li Qiang , Hu Xueyuan , Li Wei , Yang Fei , Yang Xiaolan , Sun Lili , Zhou Liping , Qi Junsheng , Yu Yu
Published: December 2009

A novel preparation of 5-oxo-5,6,7,8-tetrahydro-4 H-benzo-[b]-pyran derivatives promoted by InCl3·4H2O/TMSCl in ionic liquid ([bmin]BF4) is described. The preparative procedure presented in this paper is operationally simple and environmentally friendly. The reaction media and catalyst used can be recovered and reused for at least four times without loss in the catalytic activity. This method is promising for a mass-production process.
Synthesis of calix[4]arenes bearing benzothiazolyl, benzoxazolyl and benzoimidazolyl heterocycles
Authors: Saitz Claudio , De La Fuente Julio , Jullian Carolina , Pessoa-Mahana Hernán , Olea Carolina
Published: December 2009

A novel series of calix[4]arenes bearing benzothiazole, benzoxazole, and benzoimidazole groups were obtained by the reaction of the corresponding 2-mercaptoheterocycle with 5,11,17,23-tetra- tert-butyl-25,27-bis[2-(chloroacetamido) ethoxy]-26,28-di-hydroxycalix[4]arene and structurally characterised by IR, 1H NMR, 13C NMR, Mass spectra and elemental analyses. From their analytical data, it was found these compounds had cone conformations.
The Dimroth Rearrangement: Synthesis and Interconversion of Isomeric Triazolothienopyrimidines
Authors: Hamed Atef A. , El-Ashry El-Sayed H. , Zeid Ibrahim F. , Badr Hesham F.
Published: December 2009

Triazolo-thieno[3,2- e]pyrimidines obtained by cyclisation of 4-hydrazino-2-(methylthio)thieno[2,3- d]pyrimidine with formic acid, acetic acid, cyanogen bromide and carbon disulfide, and by oxidation of the derived aldehyde hydrazones, are found to be the triazolo[4,3- c] isomers. These [4,3- c] compounds resist isomerisation in acid, but they undergo Dimroth rearrangement to the [1,5- c] isomers under basic conditions. The crystal structure of one such rearranged product, 5-methoxy-8,9,10,11-tetrahydro[1]benzothieno[3,2- e][1,2,4]triazolo[1,5- c]pyrimidine (13b) was confirmed by X-ray analysis.
Synthesis, Crystal Structure, and Enantioseparation of a Homometallic, Chiral Cluster [Ru3(CO)9{1,2-μ-FcC(CH3) = NNC(S)NHCH3}]
Authors: Yang Jing-Mu , Hu Bin , Ge Jin , Xia Chun-Gu
Published: December 2009

Reaction of Ru3(CO)12 with the thio-Schiff base ligand acetylferrocenyl-thiosemicarbazone provides a one-step synthesis of the chiral cluster [Ru3(CO)9{1,2-μ-FcC(CH3) = NNC(S)NHCH3}] as a racemic mixture. One molecule of thiosemicarbazone was consumed in the cluster formation process, in which the ligand was deprotonated and acted as a bidentate N, S donor as well as bridging. The title cluster has been characterised by NMR, IR, HPLC and an X-ray structure determination.