Reaction of 3,5-dicyano-2,4,4,6-tetramethyl-1,4-dihydropyridine with nitric acid

1984 ◽  
Vol 49 (11) ◽  
pp. 2620-2627 ◽  
Author(s):  
Antonín Kurfürst ◽  
Josef Kuthan
Keyword(s):  
Nitric Acid ◽  
Column Chromatography ◽  
Title Compound ◽  
Mass Spectra ◽  
Probable Mechanism ◽  
Mechanism Of Formation ◽  
H Nmr ◽  
C Nmr

Reaction of the title compound I with nitric acid in acetic afforded a mixture of products which on column chromatography afforded 5-cyano-4,4,6-trimethyl-2-nitromethylene-3-oxo-1,2,3,4-tetrahydropyridine (II), (Z)-5-(1-acetoxy-2-nitrovinyl)-3,5-dicyano-4,4-dimethyl-2-pyrazoline (III) and 3-acetoxy-3-cyano-4,4,6-trimethyl-5-oxo-2,3,4,5-tetrahydropyridazine (IV). Reaction of I with nitrating mixture in chloroform gave only the compound II. The probable mechanism of formation of compounds II, III and IV, together with their 1H NMR, 13C NMR, IR and mass spectra, is discussed.

Synthesis of 2-amino-5,7-dimethyl-4-oxopyrido[3,4-e]-1,3-thiazines

1983 ◽  
Vol 48 (12) ◽  
pp. 3426-3432 ◽  
Author(s):  
Dušan Koščík ◽  
Pavol Kristian ◽  
Ondrej Forgáč
Keyword(s):  
Spectral Data ◽  
Chlorine Atom ◽  
Mass Spectra ◽  
High Reactivity ◽  
Secondary Amines ◽  
Dimroth Rearrangement ◽  
H Nmr ◽  
New Synthesis ◽  
C Nmr

New synthesis of pyrido[3,4-e]-1,3-thiazines consisting in reaction of 2,6-dimethyl-4-chloronicotinoyl isothiocyanate with primary or secondary amines, or with benzaldehyde phenylhydrazone, is described. High reactivity of the chlorine atom does not allow isolation of the corresponding thioureas, arising as intermediates, except in the case of the benzylamino derivative. Structure of the products was unequivocally confirmed by their spectral data (IR, UV, 1H NMR, 13C NMR and mass spectra). The synthesized derivatives do not undergo the Dimroth rearrangement.

Oxynemorensine, an alkaloid from Senecio nemorensis L., var. subdecurrens GRISEB

1980 ◽  
Vol 45 (2) ◽  
pp. 548-558 ◽  
Author(s):  
Antonín Klásek ◽  
Petr Sedmera ◽  
Jindřich Vokoun ◽  
Anna Boeva ◽  
Svatava Dvoráčková ◽  
...  
Keyword(s):  
Unsaturated Acid ◽  
Mass Spectra ◽  
H Nmr ◽  
C Nmr

From S. nemorensis L., var. subdecurrens GRISEB. there were isolated the previously obtained alkaloids nemorensine (I), retroisosenine (II), bulgarsenine (III) and, in addition, the alkaloid oxynemorensine which was assigned the structure VIII on the basis of the interpretation of the 1H-NMR, 13C-NMR, mass spectra, and on that of the identification of the products of hydrolysis and reduction. Furthermore, the isolation of the cis-nemorensic acid (V) as well as that of the unsaturated acid IV, and the transformation of bulgarsenine (III) to nemorensine (I) were described.

Notizen: Bis(trimethylsilylhydrazido)-thiophosphorsäurephenylester – ein neues Zwischenprodukt für die Synthese anorganischer Heterocyclen / Bis(trimethylsilylhydrazido)-thiophosphoric Acid Phenylester - A New Intermediate for the Synthesis of Inorganic Heterocycles

1975 ◽  
Vol 30 (7-8) ◽  
pp. 634-635 ◽  
Author(s):  
Lothar Steger ◽  
Udo Engelhardt
Keyword(s):  
Title Compound ◽  
Mass Spectra ◽  
Thiophosphoric Acid ◽  
H Nmr ◽  
Cis And Trans

The title compound,C6H5O-(S)P[NH-NH-Si(CH3)3]2 (1), m. p. 37-39°C, is prepared by silylation of the parent dihydrazide with (CH3)3SiCl in the presence of an excess of base. 1 is purified by vacuum destillation and characterized by 1 H NMR, IR, Ra, mass spectra and analysis. Phosphorus hydrazine heterocycles, such as cis- and trans-C6H5O-(S)P(NH-NH)2P(X)-OC6H5 (X = S, O) and others can be prepared from 1 and C6H5O-(X)PCl2 or other element dihalogene compounds.

Synthesis and reactions of substituted benzofuro[3,2-b]pyrrole derivatives

1982 ◽  
Vol 47 (12) ◽  
pp. 3288-3296 ◽  
Author(s):  
Alžbeta Krutošíková ◽  
Jaroslav Kováč ◽  
Miloslava Dandárová ◽  
Mária Bobálová
Keyword(s):  
Electron Impact ◽  
Mass Spectra ◽  
Pyrrole Derivatives ◽  
H Nmr ◽  
Electron Impact Mass ◽  
Impact Mass ◽  
C Nmr

This paper deals with the preparation of ethyl benzofuro[3,2-b]pyrrole-2-carboxylate, its hydrolysis, N-alkylation, and reduction. Also the synthesis of new heterocyclic systems, benzofuro[3,2-b]pyrrole and 2H-dihydrobenzofuro[2',3':4,5]pyrrolo[1,2-d]-1,2,4-triazin-1-one, is described. The structure of 14 new substances was corroborated by IR, UV, 1H NMR, 13C NMR and electron impact mass spectra.

Cardenolide aus Ornithogalum nutans (2 n = 28), 1. Mitteilung / Cardenolides from Ornithogalum nutans (2 n = 28), Part

1992 ◽  
Vol 47 (10) ◽  
pp. 1444-1458 ◽  
Author(s):  
Roland Ferth ◽  
Andreas Baumann ◽  
Wolfgang Robien ◽  
Brigitte Kopp
Keyword(s):  
Acid Hydrolysis ◽  
Column Chromatography ◽  
Structure Elucidation ◽  
European Species ◽  
H Nmr ◽  
First Time ◽  
Hydrolysis Of ◽  
C Nmr

From leaves and bulbs of Ornithogalum nutans L. (2 n = 28), seventeen cardenolides were isolated by column chromatography, DCCC and TLC. The structure elucidation was performed by means of 1H NMR, 13C NMR, HH-Cosy, HC-Cosy and FAB-MS studies and identification of the sugar moieties by GLC after acid hydrolysis of the cardenolides. Sugar compounds were identified as digitoxose, 3-acetyl-digitoxose, 2-deoxy-allose, 6-deoxy-allose, rhamnose, xylose and apiose. Glycosides of 7β,15β, 16 α-trihydroxy-uzarigenin, 8β,16 α-dihy-droxy, 15-oxo-uzarigenin, 3 β, 11β-dihydroxy, 12-oxo, 18-nor-5 α-card-13-enolid, 11 α-hydroxygitoxigenin, 12-oxo,8, 14β-epoxy-uzarigenin, 8β-hydroxy, 15-oxo-uzarigenin and 12β-hydroxy-oleandrigenin are described for the first time, the presence of oleandrigenin-glycosides in the genus Ornithogalum was not known until now. Ornithogalum nutans L. shows a different cardenolide pattern from the second European species of the section Myogalum (LINK) PETERM. - Ornithogalum boucheanum (KUNTH) ASCHERS.

Design, preparation and characterization of a new ionic liquid, 1,3-disulfonic acid benzimidazolium chloride, as an efficient and recyclable catalyst for the synthesis of tetrahydropyridine under solvent-free conditions

RSC Advances ◽  
2015 ◽  
Vol 5 (83) ◽  
pp. 67405-67411 ◽  
Author(s):  
Mohsen Abbasi
Keyword(s):  
Ionic Liquid ◽  
Mass Spectra ◽  
Recyclable Catalyst ◽  
Solvent Free ◽  
Disulfonic Acid ◽  
H Nmr ◽  
Solvent Free Conditions ◽  
Ft Ir ◽  
C Nmr

In the present work, 1,3-disulfonic acid benzimidazolium chloride as a new ionic liquid, is synthesized, and characterized by studying its FT-IR, 1H NMR, 13C NMR as well as mass spectra.

The Synthesis and Anticancer Activities of Peptide 5-fluorouracil Derivatives

2009 ◽  
Vol 2009 (4) ◽  
pp. 261-264 ◽  
Author(s):  
Xiaowei Yan ◽  
Maolin Hu ◽  
Qian Miao ◽  
Shun Wang ◽  
Kejian Zhao
Keyword(s):  
Cell Lines ◽  
Mass Spectra ◽  
Anticancer Activities ◽  
H Nmr ◽  
Elemental Analyses ◽  
C Nmr

A new series of peptide 5-fluorouracil derivatives was designed and synthesised in order to test in vitro anticancer activities. The results indicated that peptide 5-fluorouracil derivatives possessed anticancer activities against human HL-60 and Bel-7402 cell lines. The structures of the compounds were determined by means of 1H NMR, 13C NMR, IR, mass spectra and elemental analyses.

scholarly journals Coordination Modes of a Schiff Base Derived from Substituted 2-Aminothiazole with Chromium(III), Manganese(II), Iron(II), Cobalt(II), Nickel(II) and Copper(II) Metal Ions: Synthesis, Spectroscopic and Antimicrobial Studies

2011 ◽  
Vol 8 (4) ◽  
pp. 1750-1764 ◽  
Author(s):  
Ambit Thakar ◽  
Krishnakant Joshi ◽  
Kishor Pandya ◽  
Arvind Pancholi
Keyword(s):  
Schiff Base ◽  
Metal Ions ◽  
Transition Metal Complexes ◽  
Mass Spectra ◽  
Antibacterial Activities ◽  
Molar Conductance ◽  
Spectral Techniques ◽  
H Nmr ◽  
Antimicrobial Studies ◽  
C Nmr

Transition metal complexes of Cr(III), Mn(II), Fe(II), Co(II), Ni(II) and Cu(II) metal ions with general stoichiometry [ML2.2H2O] and [ML3], where M= Mn(II), Cr(III), Fe(II), Co(II), Ni(II) and Cu(II), L= Schiff base derived from the condensation of 2-amino-4(4’-phenyl/methylphenyl)-5-methyl-thiazole with 4-acetyl-1(3-chloro phenyl)-3-methyl-2-pyrazoline-5-ones, have been synthesized and structurally characterized by elemental analysis, molar conductance measurements, magnetic susceptibility measurements and spectral techniques like IR, UV,1H NMR,13C NMR and Mass Spectra. All the complexes were found to be octahedral geometry. The ligand and its complexes have been screened for their antifungal and antibacterial activities against three fungi,i.e. Alternaria brassicae, Aspergillus nigerandFesarium oxysporumand two bacteria,i.e. Xanthomonas compestrisandPseudomonas aeruginosa.

Synthesis and reactions of indeno[1,2-c]chromene-6,11-dione derivatives

2008 ◽  
Vol 2008 (11) ◽  
pp. 609-612 ◽  
Author(s):  
Mahmoud R. Mahmoud ◽  
Manal M. El-Shahawi ◽  
Eman A.A. El-Bordany ◽  
Fatma S.M. Abu El-Azm
Keyword(s):  
Mass Spectra ◽  
Acid Hydrazide ◽  
Sodium Hydride ◽  
Hydroxylamine Hydrochloride ◽  
Cyanoacetic Acid ◽  
H Nmr ◽  
Concentrated Sulfuric Acid ◽  
Nitrogen Nucleophiles ◽  
Cyanoacetic Acid Hydrazide ◽  
C Nmr

Indeno[1,2-c]chromene-6,11-dione was prepared using the readily obtainable starting materials via the condensation of dimethyl homophthalate with 2,6-dichlorobenzaldehyde in the presence of sodium hydride in dry benzene followed by saponification and cyclisation with concentrated sulfuric acid at 0°C. The tendency of indeno[1,2-c]chromene-6,11-dione for undergoing nucleophilic addition has been tested by reaction with nitrogen nucleophiles such as hydrazine hydrate, hydroxylamine hydrochloride, ethyl carbazate, cyanoacetic acid hydrazide, thiosemicarbazide and 4-methylbenzenesulfonohydrazide. The IR, 1H NMR, 13C NMR and mass spectra of the synthesised compounds are discussed.

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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