Heterocycles [h]-Fused onto 4-Oxoquinoline-3-carboxylic Acid. Part X [1]. Synthesis and X-Ray Structure of a Model 4- Oxo[1,4]benzoxazepino[2,3-h]quinoline-3-carboxylic Ester

2013 ◽  
Vol 68 (2) ◽  
pp. 187-194 ◽  
Author(s):  
Batool A. Farrayeh ◽  
Mustafa M. El-Abadelah ◽  
Jalal A. Zahra ◽  
Salim F. Haddad ◽  
Wolfgang Voelte
Keyword(s):  
Antifungal Activity ◽  
Carboxylic Acid ◽  
Direct Interaction ◽  
Reductive Cyclization ◽  
Carboxylic Ester ◽  
X Ray ◽  
Nmr Data ◽  
Acid Catalyzed ◽  
New Compounds ◽  
Hydrolysis Of

Direct interaction of salicylaldehyde oxyanion with ethyl 7-chloro-8-nitro-4-oxoquinoline-3- carboxylate (2) delivered the respective 7-(2-formyl-phenoxy)-8-nitro-4-oxoquinoline-3-carboxylic ester 3. Reductive cyclization of 3 furnished the corresponding 4-oxo-[1,4]benzoxazepino[2,3- h]quinoline-3-carboxylic ester 5. Acid-catalyzed hydrolysis of the esters 3/5 produced the respective acids 4/6. Structural assignments for the new compounds 3 - 6 are supported by microanalytical and spectral (IR, HRMS, NMR) data and confirmed by X-ray structure determination for compound 5. Interestingly, compound 6 exhibited good antifungal activity against C. albicans.

Isocarbostyrils. II. The Conversion of 2-Methyl-4-acyl-5-nitroisocarbostyrils to 2-Substituted Indole-4-carboxylic Acids

1971 ◽  
Vol 49 (17) ◽  
pp. 2797-2802 ◽  
Author(s):  
D. E. Horning ◽  
G. Lacasse ◽  
J. M. Muchowski
Keyword(s):  
Sulfuric Acid ◽  
Carboxylic Acid ◽  
Carboxylic Acids ◽  
Alkaline Hydrolysis ◽  
Mannich Reaction ◽  
Reductive Cyclization ◽  
Acid Catalyzed ◽  
Acid Anhydrides ◽  
Hydrolysis Of ◽  
Derivatives Of

The sulfuric acid catalyzed acylation of 2-methyl-5-nitroisocarbostyril with carboxylic acid anhydrides gave the corresponding 4-acylated derivatives 3, which underwent reductive cyclization to 2-substituted derivatives of 4-methyl-1,3,4,5-tetrahydropyrrolo[4.3.2.de]isoquinolin-5-one (4). Alkaline hydrolysis of the six-membered lactam in 4 was accompanied by a retro-Mannich reaction to produce 2-substituted indole-4-carboxylic acids in about 40 % overall yield from 3.

Synthesis of 6-Ethyl-1,2,9-trioxopyrrolo[3,2-f ]quinoline-8-carboxylic Acid

2013 ◽  
Vol 68 (5-6) ◽  
pp. 700-706 ◽  
Author(s):  
Randa M. Al-As’ad ◽  
Mustafa M. El-abadelah ◽  
Salim S. Sabri ◽  
Jalal A. Zahra ◽  
Wolfgang Voelter
Keyword(s):  
Sulfuric Acid ◽  
Carboxylic Acid ◽  
Good Yield ◽  
Chloral Hydrate ◽  
Hydroxylamine Hydrochloride ◽  
Carboxylic Ester ◽  
Nmr Data ◽  
Concentrated Sulfuric Acid ◽  
New Compounds

Interaction of 6-amino-1-ethyl-4-oxoquinoline-3-carboxylic ester (7) with chloral hydrate and hydroxylamine hydrochloride gave the corresponding isonitroso-acetamido derivative 8 which, upon treatment with concentrated sulfuric acid, was converted regioselectively into 1,2,9-trioxopyrrolo[ 3,2- f ]quinoline-8-carboxylic acid (3). This novel tricyclic system was isolated in good yield as a stable hydrate 3H. Structural assignments of the new compounds are based on microanalytical and spectral (MS and NMR) data

Solvent-free Photooxygenation of 5-methoxyoxazoles: Stereoselective Synthesis of α-amino-α-hydroxy Carboxylic Acid Derivatives

2005 ◽  
Vol 2005 (7) ◽  
pp. 422-426 ◽  
Author(s):  
Samir Bondock ◽  
Ehab Abdel Latif ◽  
Johann Lex
Keyword(s):  
Carboxylic Acid ◽  
Stereoselective Synthesis ◽  
Solid Support ◽  
Structural Elucidation ◽  
Solvent Free ◽  
X Ray ◽  
Polystyrene Beads ◽  
Hydroxy Carboxylic Acid ◽  
New Compounds ◽  
Hydrolysis Of

A solvent-free photooxygenation of 5-methoxyoxazoles 1a–j embedded in porphrin-loaded polystyrene beads as solid support is described and applied for the synthesis of 3H-1,2,4-dioxazole derivatives 2a–j. Acid catalysed hydrolysis of 3H-1,2,4-dioxazole derivatives gave α-amino-α-hydroxy carboxylic acid derivatives 3a–j. The structural elucidation of the new compounds were carried on the basis of spectral and X-ray analyses.

Tungstenmethyl-Dimethylsilanols Cp(Oc)2(R3P)W—CH2—SiMe2OH (R = Me, Ph) – Synthesis Via Oxygenation or Hydrolysis

2003 ◽  
Vol 58 (1) ◽  
pp. 36-43 ◽  
Author(s):  
Marco Hofmann ◽  
Wolfgang Malisch ◽  
Heike Hupfer ◽  
Martin Nieger
Keyword(s):  
X Ray ◽  
New Compounds ◽  
Hydrolysis Of

Abstract The tungstenmethyl-dimethylsilanols Cp(OC)2(R3P)W-CH2-SiMe2OH [R = Me (6a), Ph (6b)] have been synthesized by oxofunctionalization of the tungstenmethyl-silanes Cp(OC)2(R3P)W- CH2-SiMe2H [R = Me (3a), Ph (3b)] with dimethyldioxirane. 6a has been additionally obtained by Et3N-assisted hydrolysis of the tungstenmethyl-chlorosilane Cp(OC)2(Me3P)W-CH2- SiMe2Cl (5). Compounds 6a,b are stable with respect to self-condensation, but controlled condensation of 6a with Me2Si(H)Cl in the presence of triethylamine has been realized to give the tungstenmethyl-substituted disiloxane Cp(OC)2(Me3P)W-CH2-SiMe2O-SiMe2H (7). The new compounds have been identified IR- and NMR-spectroscopically and, in the case of 3a, by X-ray analysis.

Conditions for the formation of bayerite and gibbsite

1971 ◽  
Vol 38 (295) ◽  
pp. 358-368 ◽  
Author(s):  
W. J. Mchardy ◽  
A. P. Thomson
Keyword(s):  
Electron Microscopy ◽  
Carboxylic Acid ◽  
Electron Diffraction ◽  
Exchange Resin ◽  
Anion Exchange Resin ◽  
Acid Solutions ◽  
Salt Solutions ◽  
X Ray ◽  
Hydrolysis Of ◽  
Positively Charged

SummaryAluminium hydroxide gels have been prepared by the hydrolysis of amalgamated aluminium in water and by precipitation from aluminium salt solutions with an anion exchange resin in the hydroxyl form. The products crystallizing from such gels have been examined by electron microscopy and by X-ray and electron diffraction. Bayerite crystallizes as cone or pyramid-shaped particles and gibbsite as hexagonal plates or prisms. Two types of gel are postulated. The first type, pseudoboehmite, predominates in the absence of acids, is uncharged and rapidly crystallizes to bayerite; the second type, pregibbsite gel, occurs in carboxylic acid solutions, is positively charged and, in the absence of inorganic anions, crystallizes slowly to gibbsite.

Organophosphorverbindungen mit tertiären Alkylsubstituenten. III*: Synthese und Reaktionen Di-1-adamantylsubstituierter Phosphorverbindungen; Kristallstruktur von Di-1-Adamantylphosphinsäurechlorid / Organophosphorus Compounds with Tertiary Alkyl Substituents. Ill: Synthesis and Reactions of Di-1-adam antyl-Substituted Phosphorus Compounds; Crystal Structure of Di-1-adam antylphosphinic Chloride

1994 ◽  
Vol 49 (6) ◽  
pp. 801-811 ◽  
Author(s):  
Jens R. Goerlich ◽  
Axel Fischer ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Organophosphorus Compounds ◽  
Phosphorus Compounds ◽  
Secondary Phosphine ◽  
Phosphine Oxides ◽  
X Ray ◽  
Dry Air ◽  
Nmr Data ◽  
Standard Procedures ◽  
Hydrolysis Of ◽  
Tertiary Alkyl

The reaction of adamantane with PCl3/A1Cl3, followed by hydrolysis, gave (1-Ad)2P(:O)Cl 1, which was converted to (1-Ad)2P(:O)F 2 and (1-Ad)2P(:S)Cl 3 by standard procedures. The structure of 1 was confirmed by a single crystal X-ray structure determination; despite the bulky substituents the P-C bond lengths are normal (184.0(3), 185.0(3) pm). Whereas chlorine-fluorine exchange in 3 with AsF3 furnished (1-Ad)2P(:S)F 4, desulfuration of 3 with Ph3P to give (1-Ad)2PCl 5 failed. The secondary phosphine oxides R 1R2P(:O)H (R1, R2 = 1-Ad: 6; R1 = 1-Ad, R2 = tBu: 7; R1, R2 = tBu: 8) were synthesized by reaction of 1, 1-AdP(:O)Cl2 and tBuP(:0)Cl2 with tBuLi. 6 and 8 reacted readily with chloral to give the adducts R2P(:O)CH(OH)CCl3 (R = 1-Ad: 9; R = tBu: 10). Silylation of 6 with Me2NSiMe3 in the presence of dry air led to (1-Ad)2P(:O)OSiMe3 11, which was hydrolyzed to give (1-Ad)2P(:O)OH 12. (1-Ad)2POSiMe3 13 was obtained by the reaction of 6 with n-BuLi, followed by Me3SiCl. No reaction took place upon heating 6 with Mo(CO)6. (1-Ad)2PCl 5 was synthesized in low yield by the reaction of 6 with PCl3. The action of tetrachloro-obenzoquinone (TOB) upon 6 furnished (1-Ad)2P(:O)(o-OH)C6Cl4 15, whereas the tbutyl analogue of 15, 16, was synthesized by hydrolysis of the TOB-adduct of di-tbutylfluorophosphine. Analogous 1-adamantyl- and tbutyl-phosphorus compounds are compared with regard to their 31P NMR data

Direct Interaction of Colloidal Nanostructured ZnO and SnO2 with NO and SO2

2008 ◽  
Vol 8 (12) ◽  
pp. 6389-6397 ◽  
Author(s):  
D. Velasco-Arias ◽  
D. Díaz ◽  
P. Santiago-Jacinto ◽  
G. Rodríguez-Gattorno ◽  
A. Vázquez-Olmos ◽  
...  
Keyword(s):  
Electronic Absorption ◽  
Room Temperature ◽  
Emission Spectra ◽  
Direct Interaction ◽  
X Ray Diffraction ◽  
Wurtzite Phase ◽  
X Ray ◽  
Spontaneous Hydrolysis ◽  
Uv Visible ◽  
Hydrolysis Of

A novel and easy synthesis pathway of small SnO2 nanoparticles is reported. The method consists of the spontaneous hydrolysis of SnCl4·5H2O in dimethyl sulfoxide (DMSO), containing 3% water, at room temperature. The structure of the SnO2 nanocrystals corresponds to that of the cassiterite phase, as shown by powder X-ray diffraction and HR-TEM. The UV-visible electronic absorption and emission spectra of the SnO2 colloids are discussed. The reactions of NO(g) and SO2(g) with ZnO (wurtzite phase) and SnO2 nanocolloids are studied. The interaction of NO with ZnO nanoparticles generates the dissolution of the particles and it is quite probable that NO−13, NO−12, N2O and N2 are formed; while its contact with SO2 probably yields SO−24, SO−23 and also the dissolution of the particles is observed. When these gases are reacted with SnO2, then NO−13, NO−12, SO−23 and SO−24, were respectively obtained.

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