Calculation of 1H chemical shifts of [n]annuleno[m]annulenes and [n]annulenyl[m]annulenes

The ring current and local anisotropic contributions to the ¹H chemical shifts of [n]annuleno[m]annulenes and [n]annulenyl[m]annulenes with n, m = 12, 14, 18 and n, m = 13, 15 are calculated. The agreement between experimental and calculated shifts for the few known compounds is very good so that the predictions for the as yet unknown compounds are reliable. The effect of an annulene ring on the shifts of the protons at the other ring in these bicyclic compounds is discussed for several types of fusion of the two constituent annulenes.     

Synthesis of some new 4-imino-3,5,7-trisubstituted-pyrido[2,3-d]pyrimidine-2(1H)-thiones

The synthesis of 4-imino-3,5,7-trisubstituted-pyrido[2,3-d]pyrimidine-2(1H)-thiones is described. The elemental analysis, ir and nmr spectral data confirm the structure of the products.     

A comparative study on the synthesis of the 1H[1]benzothieno[2,3-d]-imidazole and 1H[1]benzothieno[2,3-d]-v-triazole

Alternate routes for the synthesis of the new title compounds are described. The experimental procedure for the isolation of the unstable 2,3-diaminobenzo[b]thiophene as the dichloride salt is presented.     

Crystal structure of a new complex of [3-(1 H -benzimidazol-yl)propionato- N ][3-(1 H -benzimidazol-yl) propionic acid- N ]silver(I), C20H19AgN4O4

The silver and acid hydrogen atoms in the crystal structure of [Ag(pa)(Hpa)] _n (Hpa?=?3-(1H-benzimidazol-2-yl) propionic acid-N) both lie on special positions of ?1 site symmetry; the silver atom shows linear coordination [Ag–N?=?2.109(3)?Å, N–Ag–N?=?180°]. The ‘acid hydrogen’ links molecules into a linear chain, and hydrogen bonds between the nitrogen-bound hydrogen atom and the carbonyl oxygen atom of an adjacent chain furnish a three-dimensional supramolecular structure. The compound, C₂₀H₁₉AgN₄O₄, belongs to the triclinic space group P 1 [a?=?6.536(7), b?=?8.127(9), c?=?9.051(1)?Å; α?=?81.692(2), β?=?82.819(2), γ?=?87.229(2)°], and there is one formula unit in the unit cell.     

The diphyllosilicate Rb2(VO)2[Si8O19]

Dirubidium divanadyl phyllooctasilicate, Rb₂(VO)₂[Si₈O₁₉], is the first known anhydrous diphyllosilicate containing V^IV. The structure consists of silicate double layers which are separated by [V₂O₈]⁸⁻ dimers and is related to that of the compounds A₂Cu₂[Si₈O₁₉] (A = Rb or Cs), although the title compound crystallizes in a noncentrosymmetric orthorhombic space group. The silicate double layers contain four tetrahedrally coordinated Si sites in general positions and 12 O sites, nine in general positions and the other three on mirror planes. The vanadyl dimers have two square‐pyramidally coordinated V sites (site symmetry m). There are two different 10‐ and 12‐fold coordinated Rb sites with site symmetry m, one of which is a split position located between the dimers in the interlayer space, while the other is in a channel within the silicate layer.     

Alloyed transition‐metal complexes of tricyanomethide (tcm), [Mn1−xCox(tcm)2]

Alloying in the coordination polymer [Mn_1?xCo_x(tcm)₂], (tcm = [C(CN)₃]^?) has been attempted and the physical properties have been investigated. All compounds are isostructural, but the lattice parameters and the distance between manganese and the adjacent nitrogen atom decrease with increasing cobalt content x. Magnetic susceptibility measurements show a Curie–Weiss behavior, with decreasing Weiss temperature with increasing cobalt content. Copyright © 2004 John Wiley & Sons, Ltd.     

DABCO mediated one pot synthesis of 2-(3-benzyl-2, 6-dioxo-3, 6-dihydropyrimidin-1[2H]-yl)-N-(4-(1, 3-dioxo-1H-benzo [de]isoquinolin-2[3H]-yl) aryl) acetamides as antimicrobial agents

We report herein DABCO mediated one pot synthesis of 2-(3-benzyl-2, 6-dioxo-3,6-dihydropyrimidin-1[2H]-yl)-N-(4-(1,3-dioxo-1H-benzo[de]isoquinolin-2[3H]-yl) aryl) acetamides ( 4a-j ). The silent features of this new one pot synthesis include the shorter reaction time, high yields, simple workup, and simultaneous formation of N-Amide and N-benzyl bonds in the one pot. The newly synthesized compounds ( 4a-j ) were characterized by different spectral techniques such as IR, ¹H-NMR, ¹³C-NMR, HRMS. All the synthesized compounds were evaluated for their anti-bacterial and anti-fungal activities. The anti-bacterial activities results reveal that the compounds 4a , 4g , 4i , and 4j are most active against S. aureus. In the case of B. subtilis the compounds 4a , 4i , and 4j are found to be most active. The compounds 4c , 4e , 4i , and 4j are most active against E. coli. In the case of P. aeruginosa 4a , 4i & 4j are found to be more active. On the other hand, the anti-fungal activity result shows that the compounds 4d , 4f , 4i , and 4j are more active against A. niger. The compounds 4a , 4d , 4i , and 4j are found to be more active against C. albicans.     

Syntheses of poly[N-(1-pyrenyl)acetyl ethylenimine] [pyrene-substituted linear poly(ethylenimine)] and poly[methyl 2-(1-pyrenyl)acetamidopropenoate] [pyrene-substituted poly(dehydroalanine methyl ester)]

The syntheses of two new pyrene-containing monomers—2-(1-pyrenyl)methyl-2-oxazoline ( 6 ) and methyl 2-(1-pyrenyl)acetamidopropenoate ( 12 )—and their polymerization are described. Cationic isomerization polymerization of 6 with ethylene glycol ditosylate initiator gave poly[N-(1-pyrenyl)acetyl ethylenimine] ( 7 ) and free-radical polymerization of 12 with AIBN initiator gave poly[methyl 2-(1-pyrenyl)acetamidopropenoate] ( 15 ). The monomer model compounds of the two polymers, namely, N,N-diethyl(1-pyrenyl)acetamide ( 9 ) and methyl 2-methyl-2-(1-pyrenyl)acetamidopropanoate ( 14 ), were also synthesized. The polymers were characterized by elemental analysis, IR spectroscopy, and a comparison of their ¹H-NMR spectra with those of the respective monomer model compounds.     

1H-pyrazolo[3,4-b]pyridines

The synthesis of a number of new 1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid derivatives is described. Most of these compounds have either an alkoxy or a basic substituent in position 4.     

Total assignment of the 1H NMR spectra of 5H-indolo[1,7-ab] [1]benzazepine,6,7-dihydro-5H-indolo[1,7-ab][1]benzazepine and pyrrolo[3,2,1-kl ] phenothiazine

The total assignment of the ¹H nmr spectrum of the three tetracyclic compounds: 5H -indolo[1,7-ab][1]benzazepine,6,7-dihydro-5H -indolo[1,7-ab ][1]benzazepine and pyrrolo[3,2,1-kl ]phenothiazine is described. Assignments were based on decoupling experiments and the spectrum of 1,10-dideuteriopyrrolo[3,2,1-kl]phenothiazine and the spectral parameters were verified by spin-simulation techniques. A temperature study of 6,7-dihydro-5H -indolo[1,7-ab][1]benzazepine was also performed.     

The Synthesis of Hetero-Halogenated Derivatives of Phloroglucide Analogues[1]

A short synthesis of the title compounds is reported. Most of the compounds prepared were found to be active against a number of pathogenic microorganisms in vitro.     

Multicomponent one-pot synthesis of (dihydro-1H-benzo[d]imidazole) phosphonate

Abstract

We present a multicomponent reaction strategy to synthesize a (dihydro-1H-benzo[d]imidazole)phosphonate family of compounds, using benzimidazoles, diethyl chlorophosphate and aliphatic amines as starting reactants. Giving its simplicity, our procedure involves reaction times of only few hours and avoid the usage of any catalyst agent. All the newly synthesized compounds were characterized by Nuclear Magnetic Resonance spectroscopy (¹H, ¹³C and ³¹P) and mass spectrometry by the DART method.     

Complete assignment of the 1h- and 13c-nmr spectra of [1]benzothieno[2,3-c]naphtho[1,2-h]quinoline and [1]benzothieno[2,3-c]naphtho[1,2-h][1,2,4]triazolo[4,3-a]quinoline. Concerted use of two-dimensional nmr techniques

The ¹H- and ¹³C-nmr spectra of [1]benzothieno[2,3-c]naphtho[1,2-h]quinoline and [1]benzothieno[2,3-c]-naphtho[1,2-h][1,2,4]triazolo[4,3-a]quinoline were totally assigned using a combination of two-dimensional nmr techniques. After correlation of the proton signals by a COSY spectrum and one-bond heteronuclear correlation, complete assignment of the ¹H- and ¹³C-nmr spectra of the novel heterocyclic compounds required the application of long-range CH coupling information particularly for quarternary resonance assignments and the orientations of individual spin systems relative to one another.     

The synthesis of monomethoxy[1]benzothieno[2,3-c]quinolines

A series of monomethoxy[1]benzothieno[2,3-c]quinolines 24-28 were prepared by photocylization of the appropriate 3-chloro-N-phenylbenzo[b]thiophene-2-carboxamides 9–13 to [1]benzothieno[2,3-c]quinolin-6(5H)-ones 14-18 followed by chlorination to 6-chloro[1]benzothieno[2,3-c]quinolines 19-23 then dechlorination resulting in the title compounds except for 25 which was achieved by direct reduction of 15 . Reaction of 24-28 with methyl iodide provided the corresponding N-methyl quaternary salts 29-33 . Also, conversion of 4-meth-oxy[1]benzothieno[2,3-c]quinolin-6(5H)-one 16 to 4-methoxy-6-methylthio[1]benzothieno[2,3-c]quinoline 35 and 4,6-dimethoxy[1]benzothieno[2,3-c]quinoline 36 is described.     

Sur quelques analogues fluores des [1] benzothiopyrano[4,3-b]indoles et des 6H[1] benzothiopyrano[4,3-b] quinoleines

2-, 3-, and 4-Fluorinated analogs of the carcinogenic [1]-benzothiopyrano[4,3-b]indoles and of 6H[1]benzothiopyrano-[4,3-b]quinolines have been synthesized from the corresponding fluorothiochromanones. Nmr spectral data (at 60 Mc) of the six base molecules are reported. Biological tests for the possible carcinogenic activity of these new compounds, currently under way, have already shown one of them to be a powerful sarcomagen.     

An efficient one-pot expeditious synthesis of 3-phenyl-1-(6-phenyl-7H-[1,2,4] triazolo[3,4-b] [1,3,4] thiadiazin-3-yl)-1H-pyrazol-5-amines via multicomponent approach

An efficient synthesis of 3-phenyl-1-(6-phenyl-7H-[1,2,4] triazolo[3,4-b][1,3,4]thiadiazin-3-yl)-1H-pyrazol-5-amines was accomplished by a simple, atom-economical, and multicomponent approach. Reaction of 4-amino-5-hydrazinyl-4H-1,2,4-triazole-3-thiol with various phenacyl bromides and benzoylacetonitriles in ethanol and catalytic amount of acetic acid afforded the titled compounds. The structures of newly synthesized compounds were confirmed by their analytical and spectral (IR, ¹H-NMR, ¹³C-NMR, and Mass) data.     

Bis(1-Benzyl-3,5,7-Triaza-1-Azoniatricyclo[3.3.1.13,7] Decane) Peroxodisulfate: A Mild and Efficient Oxidation of Organic Compounds Under Anhydrous and Aprotic Conditions

Bis (1-benzyl-3, 5, 7-triaza-1-azoniatricyclo[3.3.1.1^3,7] decane) perox-odisulfate was readily prepared as an white solid from commercically available hexam-ethylenetetramine and potassium peroxodisulfate. This reagent could be used as a stable, mild and efficient oxidizer to produce the corresponding carbonyl compounds from hydroxyl compounds or hydrazones or oximes and disulfides from thiols under anhydrous and aprotic conditions. The yields were almost quantitative, and the reaction time was very short.     

Luminescent 2-(hydroxyaryl)-1 H-naphth[2,3-d] imidazole derivatives

The synthesis and spectroscopic properties of a new class of luminescent 1H-naphth[2,3-d]-imidazole compounds are described. The ultraviolet spectra of 2-(hydroxyaryl)-1H-naphth[2,3-d]-imidazole derivatives are presented and discussed. Significant effects of structure and physical state of the luminescent compounds are observed on the measured emission wave length throughout the visible spectrum. The luminescence quantum efficiency of one of the naphthimidazole derivatives is reported.     

Synthesis of Some New Imidazo[4,5-B]Pyridine Derivatives Using 2-Cyanomethyl-1-Methyl-1H-Imidazo[4,5-B]Pyridine

Abstract

The reactions of 2-cyanomethyl-1-methyl-1H-imidazo[4,5-b]pyridine with isothiocyanates, nitroso compounds, acid chlorides, and thioglycolic acid were investigated. New imidazo[4,5-b]pyridine derivatives with various substituents in 2-position and derivatives of the new pyrrolo[2′,1′:2,3]imidazo[4,5-b]pyridine ring system were synthesized. The compounds obtained were tested in vitro for their tuberculostatic activity.