Identification of the condensation products of 1,2- and 1,3-amino alcohols with keto esters by NMR spectroscopy, mass spectrometry and X-ray crystallography studies. Open or ring forms?

1991 ◽  
pp. 735-741 ◽  
Author(s):  
Pirjo Vainiotalo ◽  
Pirjo-Liisa Savolainen ◽  
Markku Ahlgrén ◽  
Pentti J. Mälkönen ◽  
Jouko Vepsäläinen
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Amino Alcohols ◽  
X Ray ◽  
X Ray Crystallography ◽  
Keto Esters ◽  
Condensation Products

Synthesis and crystal structures of three novel benzimidazole/benzoindolizine hybrids

2016 ◽  
Vol 71 (3) ◽  
pp. 231-239 ◽  
Author(s):  
Roumaissa Belguedj ◽  
Sofiane Bouacida ◽  
Hocine Merazig ◽  
Ali Belfaitah ◽  
Aissa Chibani ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Dipolar Cycloaddition ◽  
Dimethyl Acetylenedicarboxylate ◽  
X Ray ◽  
X Ray Crystallography ◽  
Dimethyl Maleate

AbstractThree benzoindolizine derivatives, 1, 2, and 3, were obtained via 1,3-dipolar cycloaddition. The reaction of 1-(2′-benzimidazolylmethyl)isoquinolinium ylides with dimethyl acetylenedicarboxylate gave a mixture of pyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (1) and 1,10b-dihydropyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (2) derivatives containing a benzimidazole moiety. The reaction of this isoquinolinium N-ylide with dimethyl maleate gave an unexpected 2,3-dihydropyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (3). The structures of all reported compounds have been examined by X-ray crystallography, mass spectrometry, and NMR spectroscopy.

Synthesis, Crystal Structures, and Reactions of 2-Oxomalonylbis(arylimidoyl) Chlorides and Hydroxymethane Tris(arylimidoyl) Chlorides

2005 ◽  
Vol 58 (7) ◽  
pp. 522
Author(s):  
Richard J. Bowen ◽  
Judy Caddy ◽  
Mabel E. Coyanis ◽  
Manuel A. Fernandes ◽  
Marcus Layh ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
X Ray ◽  
X Ray Crystallography ◽  
Hydrolysis Of

The 2-oxomalonylbis(arylimidoyl) chlorides [C6H3(R2-2,6)N=CCl]2CO (R = Me, 3a; Pri, 3b; H, 3c) were synthesized from C6H3(R2-2,6)NHCHO and an excess of (COCl2)3 and their reaction with various nucleophiles was studied. Successive hydrolysis of 3a led to the formation of [C6H3(Me2-2,6)N=CCl]3COH 4a and [C6H3(Me2-2,6)NHCO]3COH 5a, while treatment of 3a with HAuCl4(H2O)x gave {[C6H3(Me2-2,6)N(H)=CCl][C6H3(Me2-2,6)NHCO]2COH}AuCl4 6a. All compounds were fully characterized by microanalysis, NMR spectroscopy, mass spectrometry, and, in the case of 3a, 4a, 5a, and 6a, by X-ray crystallography.

Synthesis, crystal structure, aggregation-induced emission (AIE) and electroluminescence properties of a novel emitting material based on pyrrolo[3,2-b]pyrrole

2020 ◽  
Vol 8 (40) ◽  
pp. 14208-14218
Author(s):  
Hongbo Wang ◽  
Jinnan Huo ◽  
Hongbo Tong ◽  
Xuehong Wei ◽  
Ying Zhang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Donor Group ◽  
Aggregation Induced Emission ◽  
X Ray ◽  
X Ray Crystallography

A novel electroluminescent material based on pyrrolo[3,2-b]pyrrole as skeleton and donor group and dimesitylborons as accept groups has been synthesized and characterized by elemental analysis, mass spectrometry, NMR spectroscopy and X-ray crystallography.

Efficient molecular ruthenium catalysts containing anionic ligands for water oxidation

2016 ◽  
Vol 45 (46) ◽  
pp. 18459-18464 ◽  
Author(s):  
Zhongkai Lu ◽  
Yan Gao ◽  
Hong Chen ◽  
Zhao Liu ◽  
Lifang Chen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Carboxylic Acid ◽  
Water Oxidation ◽  
Picolinic Acid ◽  
Ruthenium Catalysts ◽  
X Ray ◽  
X Ray Crystallography ◽  
Anionic Ligands ◽  
Ru Complexes

Two new mononuclear Ru complexes RuII(bipa)(pic)3 (1; H2bipa = 6-(1H-benzo[d]imidazol-2-yl)picolinic acid, pic = 4-picoline) and RuII(pbic)(pic)3 (2; H2pbic = 2-(pyridin-2-yl)-1H-benzo[d]imidazole-7-carboxylic acid, pic = 4-picoline) based on anionic ligands were successfully synthesized, and characterized using NMR spectroscopy, mass spectrometry, and X-ray crystallography.

scholarly journals Essential Oil and Major Non-Volatile Secondary Metabolites from the Leaves of Amazonian Piper subscutatum

Plants ◽  
2021 ◽  
Vol 10 (6) ◽  
pp. 1168
Author(s):  
Jorge Ramírez ◽  
María Daniela Andrade ◽  
Giovanni Vidari ◽  
Gianluca Gilardoni
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Secondary Metabolites ◽  
Essential Oil ◽  
Volatile Fraction ◽  
Organic Fraction ◽  
X Ray ◽  
X Ray Crystallography ◽  
Ecuadorian Amazon ◽  
First Time

The essential oil and the major non-volatile secondary metabolites from the leaves of Piper subscutatum (Miq.) C. DC. (Family Piperaceae), collected in the Ecuadorian Amazon, were analyzed for the first time in the present study. The essential oil was submitted to chemical and enantioselective analyses by GC-MS and GC-FID. (E)-β-caryophyllene (25.3–25.2%), β-chamigrene (10.3–7.8%), (E)-nerolidol (8.1–7.7%), β-selinene (7.2–7.7%), δ-cadinene (2.7–3.9%), bicyclogermacrene (3.7–2.4%), and β-pinene (2.6–3.4%) were the major components. The enantioselective analysis, carried out on a β-cyclodextrin-based column, showed four scalemic mixtures in which (1R,5R)-(+)-α-pinene, (1S,5S)-(−)-β-pinene, (S)-(−)-limonene, and (1R,2S,6S,7S,8S)-(−)-α-copaene were the major enantiomers, with enantiomeric excesses of 28.8%, 77.8%, 18.4%, and 6.0%, respectively. The study was complemented with the chemical analysis of the organic fraction dissolved in the hydrolate, whose major components were 6-methyl-5-hepten-2-one (63.7–64.4%) and linalool (6.5–6.0%). Concerning the non-volatile fraction, five lignans were the major components. (–)-Beilshminol B, (–)-grandisin, (–)-3′,4′-methylenedioxy-3,4,5-trimethoxy-7,7′-epoxylignan, (–)-3′,4′-methylenedioxy-3,4,5,5′-tetramethoxy-7,7′-epoxylignan, and (–)-3,4,3′,4′-dimethylenedioxy-5,5′-dimethoxy-7,7′-epoxylignan were identified by means of NMR spectroscopy, mass spectrometry and X-ray crystallography. The absolute configuration 7S,8S,7′S,8′S was tentatively assigned to all of them.

Water-soluble Bis(thiosemicarbazonato)copper(II) Complexes

2011 ◽  
Vol 64 (3) ◽  
pp. 244 ◽  
Author(s):  
Gojko Buncic ◽  
James L. Hickey ◽  
Christine Schieber ◽  
Jonathan M. White ◽  
Peter J. Crouch ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Cyclic Voltammetry ◽  
Nmr Spectroscopy ◽  
Cellular Uptake ◽  
Copper Complexes ◽  
Electrochemical Behaviour ◽  
Water Soluble ◽  
X Ray ◽  
X Ray Crystallography ◽  
Reversible Redox

The synthesis of four new water-soluble bis(thiosemicarbazone) ligands and their copper(ii) complexes is presented and their potential to be new ligands for copper radiopharmaceuticals is discussed. The ligands and complexes have been characterized by a combination of NMR spectroscopy, mass spectrometry, and X-ray crystallography. The electrochemical behaviour of two of the copper(ii) complexes was investigated by cyclic voltammetry and revealed that both complexes exhibited a quasi-reversible redox process attributed to a CuII/CuI process. Two of the new ligands were radiolabelled with positron-emitting 64Cu with a view to assessing their potential as ligands that bind radioactive copper isotopes for application in diagnostic radiopharmaceuticals. The cellular uptake of the copper complexes was investigated in SH-SY5Y cells.

scholarly journals Bathyptilones: Terpenoids from an Antarctic Sea Pen, Anthoptilum grandiflorum (Verrill, 1879)

Marine Drugs ◽  
2019 ◽  
Vol 17 (9) ◽  
pp. 513 ◽  
Author(s):  
Santana A.L. Thomas ◽  
Anthony Sanchez ◽  
Younghoon Kee ◽  
Nerida G. Wilson ◽  
Bill J. Baker
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Cell Line ◽  
Structure Elucidation ◽  
Two Dimensional ◽  
Mammalian Cell Line ◽  
X Ray ◽  
X Ray Crystallography ◽  
Austral Autumn ◽  
Skeleton Structure

An Antarctic coral belonging to the order Pennatulacea, collected during the 2013 austral autumn by trawl from 662 to 944 m depth, has yielded three new briarane diterpenes, bathyptilone A-C (1–3) along with a trinorditerpene, enbepeanone A (4), which bears a new carbon skeleton. Structure elucidation was facilitated by one- and two-dimensional NMR spectroscopy, mass spectrometry and confirmed by X-ray crystallography. The three compounds were screened in four cancer cell lines. Bathyptilone A displayed selective nanomolar cytotoxicity against the neurogenic mammalian cell line Ntera-2.

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