Condensation Reactions of 1,2,3,4-Tetrahydro-6-methyl-2,4-dioxo-5-pyrimidinecarbaldehyde

1995 ◽  
Vol 60 (4) ◽  
pp. 605-611 ◽  
Author(s):  
Pavel Bobáľ ◽  
Roman Gažo ◽  
Rudolf Kada ◽  
Dušan Ilavský ◽  
Naďa Prónayová ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Mass Spectra ◽  
H Nmr ◽  
Condensation Reactions ◽  
Active Methylene ◽  
Methylene Group ◽  
C Nmr

Condensation reactions of 1,2,3,4-tetrahydro-6-methyl-2,4-dioxo-5-pyrimidinecarbaldehyde with nine acid derivatives containing an active methylene group are described. The obtained products were characterized by their IR, UV, 1H NMR, 13C NMR and mass spectra. The stereochemistry of selected products was studied by 1H and 13C NMR spectroscopy.

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.

Synthesis, Characterization and Complexation Studies with K + and Ca2+ Cations of trans-1.2-Cyclohexanedioxydiacetamides

1988 ◽  
Vol 43 (2) ◽  
pp. 165-170 ◽  
Author(s):  
Whei Oh Lin ◽  
Maria C. B. V. de Souza ◽  
Helmut G. Alt
Keyword(s):  
Nmr Spectroscopy ◽  
Mass Spectroscopy ◽  
H Nmr ◽  
Coordination Sites ◽  
Complexation Studies ◽  
Ir And Nmr Spectroscopy ◽  
Elemental Analyses ◽  
C Nmr

The synthesis of trans-1.2-cyclohexanedioxydiacetamides starting with trans-1.2-cyclohexane-diol is described. Eleven of these compounds are characterized by IR, 1H NMR, 13C NMR and mass spectroscopy as well as elemental analyses. Most of these compounds are suitable ionophors for the cations K+ and Ca2+. The coordination sites of these ligands in the 1:2 complexes were determined by IR and NMR spectroscopy

[Zn(phen)2(CX3COO)]+, X = H orCl; Influence of X on the Coordination Mode of the Carboxylate Group (phen = 1,10-Phenanthroline)

2005 ◽  
Vol 60 (10) ◽  
pp. 1049-1053 ◽  
Author(s):  
Zeanab Talaei ◽  
Ali Morsali ◽  
Ali R. Mahjoub
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Coordination Mode ◽  
Bidentate Ligand ◽  
Carboxylate Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Coordinate Geometry ◽  
C Nmr

Two new ZnII(phen)2 complexes with trichloroacetate and acetate anions, [Zn(phen)2(CCl3COO)- (H2O)](ClO4) and [Zn(phen)2(CH3COO)](ClO4), have been synthesized and characterized by elemental analysis, IR, 1H NMR, 13C NMR spectroscopy. The single crystal X-ray data of these compounds show the Zn atoms to have six-coordinate geometry. From IR spectra and X-ray crystallography it is established that the coordination of the COO− group is different for trichloroacetate and acetate. The former acts as a monodentate whereas the latter acts as a bidentate ligand.

scholarly journals A Natural Triglyceride from the Methanol Root Extract of Cyphostemma Adenocaule (Steud. Ex A. Rich.) Wild & R.B.Drumm

2020 ◽  
Author(s):  
Abdulbasit Haliru Yakubu ◽  
Iliya Ibrahim ◽  
Abdulqadir bukar bababe ◽  
Hassan Yesufu ◽  
mohammed Garba Tom
Keyword(s):  
Mobile Phase ◽  
Nmr Spectra ◽  
Radical Scavenging Activity ◽  
Radical Scavenging ◽  
Solvent System ◽  
Root Extract ◽  
H Nmr ◽  
Signal Peak ◽  
Methylene Group ◽  
C Nmr

<p><i>Cyphostemma adenocaule </i>(Steud. ex A. Rich.) is one of the specie plant that belongs to the family vitacea. In this study, Trilinolein was isolated and characterized from the methanol root extract of the plant. Column chromatography over silica gel granules as the stationary phase and eluted with a mobile phase mixture of n-Hex-EtA; EtA-CHCL3 and CHCL<sub>3</sub>-MeOH with gradient increasing polarity, followed by a second column using saphadex-LH20 and 100% MeOH as stationary and mobile phase vehicle respectively. TLC was developed with EtA 15: CHCL3<sub> </sub>8: MeOH 4: H<sub>2</sub>O 1 as solvent system; sprayed with 10% H<sub>2</sub>SO<sub>4 </sub>,Vanillin-sulphuric acid, and/ or Polyethylene glycol PEG and heat for spot detection and confirmation of bioactive principles. Compound CA1 was obtained and purified with CHCL3 to give a yellow semi-solid compound (0.23g). The <sup>1</sup>H-NMR spectra showed 9 different signals; a signal peak of a glycerol (-C<b>H<sub>2</sub></b>OCOR-) moiety on the first α-C chain and on the third αʹ-C at 4.143-4.187ppm and 4.296-4.325ppm respectively, while that of a β glycerol (-C<b>H</b>COR-) at 5.286ppm. Signals of an allylic methylene group at 2.023-2.035ppm, Olefenic hydrogen group at signal peak of 5.362ppm and a diallylic methylene group at signal 2.790ppm were also observed. In the <sup>13</sup>C NMR spectra of compound CA1, 57 carbon atoms where observed, multiple signals overlapping at a range of 14.13-34.21ppm corresponding to the aliphatic CH3 (<b>C18</b>), CH2 (<b>C2, C3, C4, C5, C6, C7, C15, C16, and C17</b>) and allylic (<b>C8, C14</b>) carbon atoms. Signals at 127.90-130.24ppm were assigned to the olefienic C atoms (<b>C9, C10, C12</b>, and <b>C13</b>) while signal of 172.87ppm and 173.32ppm were assigned to the carbonyl (<b>C</b>=O) carbon atoms (<b>C1 </b>and<b> C2</b>) respectively (Table 2). </p> <p>Analysis with DEPT-135, H-H COSY, HMBC and HSQC assignments of CA1 augments assignment of signals made for CA1 from <sup>1</sup>H-NMR and <sup>13</sup>C-NMR and corresponded to that of Trilinolein <u>(<a href="https://pubchem.ncbi.nlm.nih.gov/#query=C57H98O6">C<sub>57</sub>H<sub>98</sub>O<sub>6</sub></a>, </u>MW 879.4 g/mol). The isolated compound was positive for the acrolein test for triglycerides; fat & oil and had an IC<sub>50</sub> of 46.08µg/ml radical scavenging activity.</p>

scholarly journals Three-Dimensional Supramolecular Network Directed by Intermolecular Interactions in [Pb2(dmp)2(hfacac)4]

2009 ◽  
Vol 6 (4) ◽  
pp. 1085-1090
Author(s):  
Farzin Marandi ◽  
Lotfali Saghatforoush ◽  
Hossein Farzaneh
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Three Dimensional ◽  
Supramolecular Network ◽  
Stacking Interactions ◽  
H Nmr ◽  
Noncovalent Bond ◽  
Donor And Acceptor ◽  
Anionic Ligands ◽  
C Nmr

To investigate the interactions between noncovalent bond donor and acceptor giving rise to three dimensional networks, compound [Pb2(dmp)2(hfacac)2] (1) (dmp = 2,9-dimethyl-1,10-henanthroline and Hhfacac = hexafluoroacetylacetonate) has been prepared and characterized by elemental analysis, IR,1H NMR, and13C NMR spectroscopy and its crystal structures was investigated. The single crystal structure show the coordination number of Pb(II) to be eight with twoN-donor atoms from a “dmp” ligand and sixO-donors from the anionic ligands. The supramolecular structure of 1 is realized by weak directional C–H∙∙∙O–C, C–F∙∙∙F–C andπ–πstacking interactions.

Synthesis and Pharmacological Activities of Some New 2-[1-Heptyl-3-(4- methoxybenzyl)-5-oxo-1,5-dihydro-4H-1,2,4-triazol-4-yl]acetohydrazide Derivatives

2014 ◽  
Vol 69 (9-10) ◽  
pp. 969-981 ◽  
Author(s):  
Olcay Bekircan ◽  
Emre Mentese ◽  
Serdar Ulker
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Lipase Activity ◽  
Spectral Studies ◽  
Antituberculosis Activity ◽  
Pharmacological Activities ◽  
Mass Spectral ◽  
H Nmr ◽  
Acetohydrazide Derivative ◽  
C Nmr

Abstract In the present investigation, the key intermediate acetohydrazide derivative 5 was synthesized starting from 3-(4-methoxybenzyl)-4-amino-4,5-dihydro-1,2,4-triazol-5-one (1) by a four-step reaction. Thiosemicarbazides 6a-f and arylidenehydrazide derivatives 8a-d were obtained from compound 5. The cyclization of compounds 6a-f in the presence of NaOH resulted in the formation of compounds 7a-f. The compounds were characterized by IR, 1H NMR, 13C NMR spectroscopy, elemental analysis and mass spectral studies. The compounds were tested for their anti-lipase, anti-α-glucosidase and anti-mycobacterial activities. Compounds 6b and 8c exhibited excellent anti-lipase activity, and compound 8d showed excellent anti-a-glucosidase activity. Compounds 3 and 4 exhibited good antituberculosis activity

scholarly journals Synthesis of cis, cis-1,3,5-trisubstituted cyclohexane based chelators with polyfunctional pendant arms

2005 ◽  
Vol 2005 (1) ◽  
pp. 43-45 ◽  
Author(s):  
Minati Baral ◽  
B.K. Kanungo ◽  
Peter Moore
Keyword(s):  
Schiff Base ◽  
Nmr Spectroscopy ◽  
Organic Compounds ◽  
Elemental Analysis ◽  
H Nmr ◽  
Benzenetricarboxylic Acid ◽  
New Compounds ◽  
Pendant Arms ◽  
C Nmr

Some novel organic compounds of the type: cis, cis-1,3,5-tris(X)cyclohexane, where X= –CONH(CH2)2NH2, –CONH(CH2)3NH2, –CONH(CH2)2NCH –C6H4OH, CONH(CH2)3NCHC6H4OH, which are expected to function as potential polydentate chelators have been synthesised from 1,3,5-benzenetricarboxylic acid through multi-steps reactions. 1,3,5-benzenetricarboxylic acid was reduced to cis, cis-1,3,5-tris(ethylcarboxylate)cyclohexane, which on reaction with excess of 1,2-diaminoethane and 1,2-diaminopropane afforded two new compounds. Condensation of the obtained derivatives with three equivalents of salicylaldehyde resulted the formation of two new Schiff base compounds. All the compounds were characterised by a combination of elemental analysis, mass, IR, UV-Vis, 1H NMR and 13C NMR spectroscopy.

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.

scholarly journals Isomeric Di-C-glycosylflavones in Fig (Ficus carica L.)

1985 ◽  
Vol 40 (1-2) ◽  
pp. 8-12 ◽  
Author(s):  
Fred Siewek ◽  
Karl Herrmann ◽  
Lutz Grotjahn ◽  
Victor Wray
Keyword(s):  
Nmr Spectroscopy ◽  
Reversed Phase ◽  
Ficus Carica ◽  
Preparative Hplc ◽  
H Nmr ◽  
Gradient Hplc ◽  
C Nmr

Two isomeric C-glycosides of apigenin (apigenin-6-C-glucosyl-8-C-arabinoside (schaftoside), apigenin-6-C-arabinosyl-8-C-glucoside (isoschaftoside)) were isolated from leaves of Ficus carica with preparative HPLC. 1The glycosides were identified by UV-, 1H-NMR-, 13C-NMR-spectroscopy and FAB-MS. Their concentration in fruits and leaves were determined by gradient HPLC on reversed phase material.

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