Zirconium(IV) chloride-catalyzed synthesis of 1,5-benzodiazepine derivatives

2007 ◽  
Vol 85 (3) ◽  
pp. 184-188 ◽  
Author(s):  
K Srinivasa Reddy ◽  
Ch. Venkateshwar Reddy ◽  
M Mahesh ◽  
K Rosi Reddy ◽  
P VK Raju ◽  
...  
Keyword(s):  
Structural Elucidation ◽  
High Yield ◽  
Zirconium Tetrachloride ◽  
H Nmr ◽  
Cyclocondensation Reaction ◽  
Benzodiazepine Derivatives

Zirconium tetrachloride efficiently catalyzes the cyclocondensation reaction of o-phenylenediamine and a ketone in refluxing 1,2-dichloroethane to afford the corresponding 2,3-dihydro-1H-1,5-benzodiazepine in high yield. The formation of specific regioisomers and their structural elucidation are reported for the first time.Key words: zirconium tetrachloride, o-phenylenediamines, ketones, 1,5-benzodiazepines, 1H NMR, regioisomers.

Nine- and Eight-Vertex Polyhedral Dicarbaborane Chemistry: New arachno and hypho Dicarbaboranes from arachno-4,5-C2B7H13: Isolation and Characterization of the [arachno-4,5-C2B7H12]- and [hypho-7,8-C2B6H13]- Anions, and of the Neutral Ligand Derivatives exo-6-(MeNC)-arachno-4,5-C2B7H11 and exo-5-L-hypho-4,9-C2B7H13 (L = NMe3 and NEt3)

1994 ◽  
Vol 59 (7) ◽  
pp. 1584-1595 ◽  
Author(s):  
Tomáš Jelínek ◽  
Josef Holub ◽  
Bohumil Štíbr ◽  
Xavier L. R. Fontaine ◽  
John D. Kennedy
Keyword(s):  
Nmr Spectroscopy ◽  
Selective Removal ◽  
High Yield ◽  
Two Dimensional ◽  
Neutral Ligand ◽  
Tertiary Amines ◽  
Proton Sponge ◽  
H Nmr ◽  
Isolation And Characterization

Deprotonation of neutral arachno-4,5-C2B7H13 (1) either with 1, 8-(NMe2)2C10H6 (proton sponge, PS) or with a mixture of aqueous K2CO3 and [NMe4]Cl leads to the isolation in high yield of the [arachno-4,5-C2B7H12]- anion (2). Isostructural with this anion is the ligand derivative exo-6-(MeNC)-arachno-4,5-C2B7H11 (3), which is prepared in 20% yield from the reaction between arachno-4,5-C2B7H13 and MeNC in dichloromethane. Under comparable conditions compound 1 with tertiary amines gives the first representatives of the nine-vertex hypho family of dicarbaboranes, the ligand derivatives exo-5-(NR3)-hypho-4,9-C2B7H13 (4a and 4b, where R = Me and Et, respectively) in moderate yields (20 - 55%), whereas the reaction between 1 and aqueous NaCN results in the selective removal of one boron vertex to yield the eight-vertex [hypho-7,8-C2B6H13]- anion (5) in 61% yield. All compounds isolated were characterized by 11B and 1H NMR spectroscopy, with two-dimensional and selective decoupling techniques giving unambiguous assignments.

scholarly journals A High-Yield Synthesis of Chalcopyrite CuInS2Nanoparticles with Exceptional Size Control

2009 ◽  
Vol 2009 ◽  
pp. 1-7 ◽  
Author(s):  
Chivin Sun ◽  
Joseph S. Gardner ◽  
Endrit Shurdha ◽  
Kelsey R. Margulieux ◽  
Richard D. Westover ◽  
...  
Keyword(s):  
Microwave Irradiation ◽  
Size Control ◽  
High Yield ◽  
Single Source ◽  
Icp Oes ◽  
Single Source Precursors ◽  
H Nmr ◽  
High Yields ◽  
Size Controlled

We report high-yield and efficient size-controlled syntheses of Chalcopyrite CuInS2nanoparticles by decomposing molecular single source precursors (SSPs) via microwave irradiation in the presence of 1,2-ethanedithiol at reaction temperatures as low as 100°C and times as short as 30 minutes. The nanoparticles sizes were 1.8 nm to 10.8 nm as reaction temperatures were varied from 100°C to 200°C with the bandgaps from 2.71 eV to 1.28 eV with good size control and high yields (64%–95%). The resulting nanoparticles were analyzed by XRD, UV-Vis, ICP-OES, XPS, SEM, EDS, and HRTEM. Titration studies by1H NMR using SSP1with 1,2-ethanedithiol and benzyl mercaptan were conducted to elucidate the formation of Chalcopyrite CuInS2nanoparticles.

scholarly journals Synthesis and Structural Elucidation of the Acetylation Reaction’s Product(s) of the 2(1H)-Quinoxalinones Derived from L-Ascorbic Acid. X-Ray Molecular Structure of 3-(N-acetyl-2-naphthylhydrazono)-2,3-dihydro-2-acetoxyfuro[2,3-b]quinoxaline [1]

1992 ◽  
Vol 47 (6) ◽  
pp. 861-868 ◽  
Author(s):  
Adel Amer ◽  
Douglas M. Ho
Keyword(s):  
Molecular Structure ◽  
Ascorbic Acid ◽  
Acetic Anhydride ◽  
Structural Elucidation ◽  
Ring Closure ◽  
The Other ◽  
High Yield ◽  
X Ray ◽  
Reaction Condition ◽  
Tricyclic Compound

Acetylation reaction’s product(s) of 3-[L-threo-2,3,4-trihydroxy-1-(2-naphthylhydrazono)-butyl]quinoxalin-2(1H)-one (2b) were found to be dependent on the reaction condition. While the tri-O-acetyl (3b) was isolated in high yield from 2b under the action of acetic anhydride/pyridine mixture, compounds 4b and 5b as well as trace of 3b were obtained when 2b was heated in acetic anhydride. On the other hand, 3-[1-(2-naphthylhydrazono)-glyoxal-1-yl]quinoxalin-2(1H)-one (7) underwent ring closure and afforded the condensed tricyclic compound 8 under the action of acetic anhydride/pyridine mixture.

Preparation and Crystal Structure of Genistein Benzenesulfonate Prodrugs

2008 ◽  
Vol 2008 (10) ◽  
pp. 555-558 ◽  
Author(s):  
You Peng ◽  
Zeyuan Deng ◽  
Shaojie Lang ◽  
Yawei Fan
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Sulfonic Acid ◽  
Nmr Spectra ◽  
High Yield ◽  
X Ray Diffraction ◽  
Aromatic Rings ◽  
X Ray ◽  
H Nmr ◽  
Ester Prodrugs

In order to improve bioavailability and anticancer activity of genistein, a series of novel sulfonic acid ester prodrugs of the isoflavone genistein were synthesised in high yield with excellent regioselectivity. Their structures were characterised by IR, MS, elemental analysis and 1H NMR spectra. The crystal structure was examined by X-ray diffraction. X-ray structure determination revealed that all the aromatic rings in the compound are not coplanar. In the crystal structure, molecules are linked through intermolecular C-H···O hydrogen bonds, forming layers parallel to the ab plane.

Synthesis of Triferrocenylbenzenes by Tantalum(V)-Catalyzed Cyclotrimerization of Ethynylferrocene. The Crystal Structure of 1,3,5-Triferrocenylbenzene

1997 ◽  
Vol 62 (10) ◽  
pp. 1577-1584 ◽  
Author(s):  
Petr Štěpnička ◽  
Ivana Císařová ◽  
Jan Sedláček ◽  
Jiří Vohlídal ◽  
Miroslav Polášek
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystal ◽  
High Yield ◽  
Isomer Mixture ◽  
State Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Yield Formation

Exclusive, high-yield formation of the cyclotrimers of ethynylferrocene (1) was observed when TaCl5 in benzene was employed as catalyst. Analysis of the resulting isomer mixture by means of HPLC and 1H NMR revealed the presence of 1,3,5-triferrocenylbenzene (sym-2) and 1,2,4-triferrocenylbenzene (asym-2) in the ratio of 4 : 6. A small amount of pure sym-2 isomer was isolated, and its solid-state structure was established by single-crystal X-ray diffraction. The molecules of sym-2 possess a distorted up-up-down arrangement of the ferrocenyl groups attached to the benzene ring.

scholarly journals Zinc Oxide Nanoparticles Catalyzed Condensation Reaction of Isocoumarins and 1,7-Heptadiamine in the Formation of Bis-Isoquinolinones

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Varadhan Krishnakumar ◽  
Kesarla Mohan Kumar ◽  
Badal Kumar Mandal ◽  
Fazlur-Rahman Nawaz Khan
Keyword(s):  
Zinc Oxide ◽  
Zinc Oxide Nanoparticles ◽  
Condensation Reaction ◽  
High Yield ◽  
Oxide Nanoparticles ◽  
Acid Chlorides ◽  
Zno Nps ◽  
H Nmr ◽  
Yield And Purity ◽  
C Nmr

The diversified bis-isoquinolinones were obtained in two steps, utilizing homophthalic acid and various acid chlorides providing 3-substituted isocoumarins in the first step which on further condensation with 1,7-heptadiamine involving C–N bond formation from the lactone in the presence of 10 mol% zinc oxide nanoparticles (ZnO NPs) (<150 nm) afforded the desired bis-isoquinolinones in high yield and purity. The synthesized compounds were then characterized using FTIR,1H NMR,13C NMR, and HRMS techniques.

Synthesis and Characterization of Ionic Liquid 1-Propargly-3-Methylimidazolium Chlorate

2012 ◽  
Vol 427 ◽  
pp. 173-178
Author(s):  
Ying Jie Cai ◽  
Xiu Jie Ji ◽  
Bo Wen Cheng ◽  
Dong Dong Xie ◽  
Qiu Ling Wang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ionic Liquid ◽  
Structure Analysis ◽  
Crystal Structure Analysis ◽  
High Yield ◽  
Imidazolium Ionic Liquid ◽  
H Nmr ◽  
Compound C ◽  
And Function ◽  
Relationship Of

The title compound (C7H9ClN2, Mr = 156.61), an imidazolium ionic liquid with alkynyl, was synthesized by an improved method in high yield. FT-IR,1H NMR,13C NMR and elemental analysis were performed to characterize the molecule of the ionic liquid, and its crystal structure was determined by single-crystal X-ray structure analysis. The results indicate that the improved procedure is very feasible and 96% yield. The crystal structure analysis will be conducive to clarify the relationship of structure and function for ionic liquid with alkynyl the compound.

Cycloheptatriene dimers: New precursors of diamantane

1981 ◽  
Vol 46 (6) ◽  
pp. 1474-1485 ◽  
Author(s):  
František Tureček ◽  
Vladimír Hanuš ◽  
Petr Sedmera ◽  
Helena Antropiusová ◽  
Karel Mach
Keyword(s):  
Mass Spectra ◽  
High Yield ◽  
Stable Isomer ◽  
Titanium Complexes ◽  
H Nmr ◽  
Catalytic Isomerization ◽  
C Nmr

Dimerization of cycloheptatriene, catalyzed by titanium complexes, afforded pentacyclo[8.4.0.03,7.04,14.06,11]tetradeca-8,12-diene (I) (10%) and pentacyclo[7.5.0.02,8.05,14.07,11]tetradeca-3,12-diene (II) (90%). Structure of both dimers and their derivatives was determined by means of 1H NMR, 13C NMR and mass spectra. On heating, the diene II was converted into the more stable isomer I. On hydrogenation and further catalytic isomerization, both I and II gave diamantane in high yield.

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