Reaction of O-Alkyl-N-substituted Iminothiocarbonates with Bromoacetyl Bromide. A General Method for the Synthesis of 3-Substituted 1,3-Thiazolidine-2,4-diones

1996 ◽  
Vol 61 (3) ◽  
pp. 432-436 ◽  
Author(s):  
Ján Imrich ◽  
Juraj Bernát ◽  
Pavol Kristian ◽  
Tatiana Bušová ◽  
Slávka Hočová
Keyword(s):  
Mass Spectroscopy ◽  
High Purity ◽  
Sodium Salts ◽  
H Nmr ◽  
Independent Synthesis ◽  
General Method ◽  
C Nmr

Reaction of sodium salts of O-methyl-N-substituted iminothiocarbonates with bromoacetyl bromide represents a new general method for preparation of 3-substituted 1,3-thiazolidine-2,4-diones in good yields and high purity. The structure of the synthesized products has been confirmed by 1H NMR, 13C NMR, IR and mass spectroscopy as well as by independent synthesis.

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

scholarly journals Synthesis of compounds related to the anti-migraine drug eletriptan hydrobromide

2012 ◽  
Vol 8 ◽  
pp. 1400-1405 ◽  
Author(s):  
Suri Babu Madasu ◽  
Nagaji Ambabhai Vekariya ◽  
M N V D Hari Kiran ◽  
Badarinadh Gupta ◽  
Aminul Islam ◽  
...  
Keyword(s):  
Mass Spectroscopy ◽  
Acute Treatment ◽  
Selective Serotonin ◽  
Spectroscopic Techniques ◽  
Active Pharmaceutical Ingredients ◽  
Pharmaceutical Ingredients ◽  
H Nmr ◽  
Related Compounds ◽  
C Nmr ◽  
Anti Migraine Drug

Eletriptan hydrobromide (1) is a selective serotonin (5-HT1) agonist, used for the acute treatment of the headache phase of migraine attacks. During the manufacture of eletriptan hydrobromide the formation of various impurities were observed and identified by LC–MS. To control the formation of these impurities during the preparation of active pharmaceutical ingredients, the structure of the impurities must be known. Major impurities of the eletriptan hydrobromide synthesis were prepared and characterized by using various spectroscopic techniques, i.e., mass spectroscopy, FTIR , 1H NMR, 13C NMR/DEPT, and further confirmed by co-injection in HPLC. The present study will be of great help in the synthesis of highly pure eletriptan hydrobromide related compounds.

Synthesis and Characterization of Imidazo[1,2-a]Pyrimidine

2015 ◽  
Vol 52 ◽  
pp. 1-4
Author(s):  
A.M. Shah ◽  
A.J. Rojivadiya
Keyword(s):  
Mass Spectroscopy ◽  
Synthesis And Characterization ◽  
Spectroscopic Techniques ◽  
One Pot ◽  
H Nmr ◽  
Ft Ir ◽  
C Nmr

An efficient protocol for the synthesis of imidazo [1,2-a] pyrimidine was developed by using three component one-pot Biginelli synthesis. The synthesized compounds were characterized by spectroscopic techniques like FT-IR, 1H NMR, 13C NMR, and mass spectroscopy.

Catalytic epoxidation of stilbenes with non-peripherally alkyl substituted carbonyl ruthenium phthalocyanine complexes

2012 ◽  
Vol 16 (04) ◽  
pp. 403-412 ◽  
Author(s):  
Charles A. Enow ◽  
Charlene Marais ◽  
Barend C.B. Bezuidenhoudt
Keyword(s):  
Catalytic Activity ◽  
Mass Spectroscopy ◽  
High Catalytic Activity ◽  
H Nmr ◽  
Catalytic Epoxidation ◽  
Metal Insertion ◽  
New Compounds ◽  
C Nmr

A number of novel carbonyl(1,4,8,11,15,18,22,25-octaalkylphthalocyaninato)-ruthenium(II) complexes were prepared by metal insertion with Ru3(CO)12. The new compounds have been characterized by1H NMR,13C NMR, IR, UV-vis and mass spectroscopy. This study demonstrated that this type of complexes and specifically carbonyl(1,4,8,11,15,18,22,25-octahexylphthalo-cyaninato)ruthenium(II) and carbonyl[1,4,8,11,15,18,22,25-octa(2-cyclohexylethyl)phthalocyaninato]-ruthenium(II), exhibit high catalytic activity and stability in the epoxidation of stilbenes with 2,6-dichloropyridine N-oxide as oxidant.

New Preparation of 2-N-Alkyl(aryl)amino-5-methyl-4H-1,3-thiazin-4-ones and 3,4-Dihydro-5-methyl-2,4-dioxo-2H-1,3-thiazine

1993 ◽  
Vol 58 (4) ◽  
pp. 893-901 ◽  
Author(s):  
Dušan Koščík ◽  
Milan Dzurilla ◽  
Peter Kutschy
Keyword(s):  
Mass Spectroscopy ◽  
Secondary Amines ◽  
Addition Reactions ◽  
Cyclization Reactions ◽  
Alkyl Aryl ◽  
New Approach ◽  
H Nmr ◽  
Primary And Secondary Amines ◽  
Sole Product ◽  
C Nmr

Addition-cyclization reactions of 3-bromo- and 3-chloro-2-methylpropenoylisothiocyanates with primary and secondary amines and alcohols have been studied. The formed addition products, thioureas, underwent cyclization of heating with ethanolic KOH or in dimethylformamide in the presence of lithium hydride. This method represents a new approach to 2-dialkyl(aryl)amino-5-methyl-4H-1,3-thiazin-4-ones. Addition reactions with alcohols afforded 3,4-dihydro-5-methyl-2,4-dioxo-2H-1,3-thiazine as the sole product. The structure of the synthesized compounds was confirmed by 1H NMR, 13C NMR, IR and mass spectroscopy.

Syntheses of New Triethylene Glycol Bis(alkyl Phosphate)s as Potential Complexing Agents

2001 ◽  
Vol 66 (4) ◽  
pp. 621-630 ◽  
Author(s):  
Věra Novoměstská ◽  
Eckhard Herrmann ◽  
Přemysl Lubal ◽  
Jiří Příhoda
Keyword(s):  
Ir Spectroscopy ◽  
Mass Spectroscopy ◽  
Elemental Analysis ◽  
Metal Cations ◽  
Triethylene Glycol ◽  
Complexing Agents ◽  
H Nmr ◽  
Maldi Tof ◽  
Alkyl Phosphate ◽  
C Nmr

A series of triethylene glycol bis(alkyl phosphate)s HO(RO)P(O)(OCH2CH2)3OP(O)(OR)OH 4 (R = octyl (4a), 1-methylheptyl (4b), 2-ethylhexyl (4c), nonyl (4d), decyl (4e), dodecyl (4f), hexadecyl (4g), octadecyl (4h)) has been synthesized with the expectation that these compounds could be effective complexing and/or extraction agents for metal cations. The compounds were characterized by 31P NMR, 1H NMR, 13C NMR and IR spectroscopy, MALDI-TOF mass spectroscopy and elemental analysis.

Synthesis of 1,3-diazaspiro[5,5]undecanes and 1-thia-3-azaspiro[5,5]undec-2-enes by reaction of 2-cyanocyclohexylideneacetyl isothiocyanate with amines and sodium hydrogen sulfide

1987 ◽  
Vol 52 (4) ◽  
pp. 989-994 ◽  
Author(s):  
Milan Dzurilla ◽  
Ondrej Forgáč ◽  
Peter Kutschy ◽  
Pavol Kristian ◽  
Dušan Koščík ◽  
...  
Keyword(s):  
Hydrogen Sulfide ◽  
Alkaline Medium ◽  
Mass Spectroscopy ◽  
Aromatic Amines ◽  
Secondary Amines ◽  
H Nmr ◽  
Sodium Hydrogen ◽  
Elemental Analyses ◽  
Primary Aromatic Amines ◽  
C Nmr

2-Cyanocyclohexylideneacetyl isothiocyanate (II) reacts with sodium hydrogen sulfide to give 1-thia-3-azaspiro[5,5]undecane. Reaction of II with secondary amines afforded 1-thia-3-azaspiro[5,5]undec-2-enes whereas primary aromatic amines gave 1,3-diazaspiro[5,5]undecanes under the same conditions. Both types of reactions proceed via substituted thioureas which were isolated pure only in the case of 4-methylaniline and 4-methoxyaniline. They were cyclized in alkaline medium to the corresponding diazaspiro derivatives. The structure of the synthesized compounds was confirmed by their elemental analyses and IR, 1H NMR, 13C NMR and mass spectroscopy.

“Turn-on” fluorescent chemosensor for zinc(ii) dipodal ratiometric receptor: application in live cell imaging

2014 ◽  
Vol 13 (7) ◽  
pp. 1052-1057 ◽  
Author(s):  
Kundan Tayade ◽  
Banashree Bondhopadhyay ◽  
Hemant Sharma ◽  
Anupam Basu ◽  
Vikas Gite ◽  
...  
Keyword(s):  
Mass Spectroscopy ◽  
Live Cell Imaging ◽  
Cell Imaging ◽  
Condensation Reaction ◽  
Live Cell ◽  
Fluorescent Chemosensor ◽  
H Nmr ◽  
Turn On ◽  
C Nmr

A dipodal ligand 2,2′-((ethane-1,2-diylbis(azanediyl))bis(ethane-1,1-diyl))diphenol was synthesized through a condensation reaction and was characterized with IR, 1H NMR, 13C-NMR, and mass spectroscopy.

Reactions of 11-chloro-11-phenyl-6,11-dihydrodibenzo[b,e]-thiepin with piperidine and some further nucleophiles

1982 ◽  
Vol 47 (11) ◽  
pp. 3094-3113 ◽  
Author(s):  
Miroslav Protiva ◽  
Karel Šindelář ◽  
Vladimír Valenta ◽  
Jiří Holubek ◽  
Emil Svátek ◽  
...  
Keyword(s):  
Methyl Derivative ◽  
Substitution Product ◽  
Normal Product ◽  
H Nmr ◽  
Independent Synthesis ◽  
The One ◽  
Neurotropic Effects ◽  
Derivatives Of ◽  
C Nmr

The title compound Vb affords with piperidine normal nucleophilic substitution product and the isomeric 3-piperidino derivative XXXII. The structure of XXXII was proven by (1) the 1H NMR and 13C NMR spectra, (2) an independent synthesis via the intermediates XXXV, XXXVI, XXX, IV and VIIIa, and (3) with the help of model reactions of the 2-methyl derivative VIb and the 3-methyl derivative VIIb with piperidine. The rearranged cation XXXVII is considered a precursor of the product XXXII. Similar mixtures are apparently formed in reactions of the chloro derivative Vb with a series of further amines where, however, mostly the normal substitution products (XV-XXI) were isolated and only in two cases the formation of the 3-substituted compounds (XXXIII, XXXIV) was noted. The 11-amino derivatives of the type XIII are unstable in ethanol in the presence of hydrogen chloride; the product of their acid catalyzed solvolysis is the ethoxy derivative XIV. Potassium phthalimide reacts with the compound Vb under the formation of the normal product XXII accompanied by 9-phenylanthracene (XXXVIII). Reaction of Vb with 3-dimethylaminopropylmagnesium chloride affords on the one hand the normal product XXIV, and the isomer on the other, to which the structure XXXIX is ascribed. The biological screening of the amines prepared showed with some compounds a rather significant antimicrobial activity in vitro (e.g. XXXIII) and some structurally less specific neurotropic effects, especially the spasmolytic (XXII, XXXIX) and the central depressant one (XX, XXXIII).

5aH.10aH.15aH-Tribenzo [b.f.j] [1.4.7] trioxa [9 b] azaphenalene - vermeintliche Benzoxete / 5aH, 10aH, 15aH-Tribenzo[b,f,j][l,4,7]trioxa[9 b]azaphenalenes - Supposed Benzoxetes

1979 ◽  
Vol 34 (2) ◽  
pp. 290-296 ◽  
Author(s):  
Herbert Meier ◽  
Ahmed Issa ◽  
Ursula Merkle
Keyword(s):  
Alkaline Medium ◽  
Mass Spectroscopy ◽  
Structure Elucidation ◽  
H Nmr ◽  
Degradation Reactions ◽  
Polycyclic System ◽  
C Nmr

Abstract A supposed benzoxete is determined as a complex polycyclic system: cis,cis,cis-5 aH,10 aH,15 aH-tribenzo[b,f,j][1,4,7]trioxa[9 b]azaplienalene. The structure elucidation is performed by spectroscopycal methods (IR, 1H NMR, 13 C NMR and mass spectroscopy) and by degradation reactions in an acidic or an alkaline medium.

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