A New Dimeric Derivative of Ethoxyquin from Its Reaction with Alkylperoxy Radicals

1993 ◽  
Vol 58 (8) ◽  
pp. 1914-1918 ◽  
Author(s):  
Jaroslav Kříž ◽  
Luděk Taimr
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Peroxy Radicals ◽  
Methyl Group ◽  
Alkylperoxy Radicals ◽  
C Nmr

The structure of a new compound formed in the reaction of ethoxyquin with alkylperoxy radicals was resolved by 1H and 13C NMR spectroscopy (including COSY, NOESY, HHC RCT and SSLR INEPT techniques) and confirmed by mass spectrometry. The structure suggest participation of 4-methyl group of ethoxyquin in the deactivation of peroxy radicals. A mechanism of this reaction is proposed.

The mechanism of formation of 2,7-dimethyl-2,6-octadiene in the synthesis of 3-methylene-7-methyl-1,6-octadiene

1983 ◽  
Vol 48 (7) ◽  
pp. 1864-1866
Author(s):  
Jan Bartoň ◽  
Ivan Kmínek
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Alkali Metal ◽  
Chromatographic Analysis ◽  
Solid Phase ◽  
Reaction Pathway ◽  
Mechanism Of Formation ◽  
Gas Chromatographic Analysis ◽  
C Nmr ◽  
Visual Observations

2,7-Dimethyl-2,6-octadiene is formed in the catalytic solution for the dimerization of 2-methyl-1,3-butadiene to β-myrcene (3-methylene-7-methyl-1,6-octadiene), as revealed by mass spectrometry and 13C NMR spectroscopy. Visual observations together with the results of gas chromatographic analysis of the catalytic solution suggest that the formation of 2,7-dimethyl-2,6-octadiene is associated with the transition of the alkali metal (sodium) from the solid phase into the solution. A reaction pathway is suggested accounting for the formation of 2,7-dimethyl-2,6-octadiene in the system.

scholarly journals A switchable [2]rotaxane with two active alkenyl groups

2018 ◽  
Vol 14 ◽  
pp. 2074-2081 ◽  
Author(s):  
Xiu-Li Zheng ◽  
Rong-Rong Tao ◽  
Rui-Rui Gu ◽  
Wen-Zhi Wang ◽  
Da-Hui Qu
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Functional Groups ◽  
Stimuli Responsive ◽  
Stimuli Responsive Polymers ◽  
Responsive Polymers ◽  
Recognition Sites ◽  
Acid And Base ◽  
C Nmr

A novel functional [2]rotaxane containing two alkenyl bonds was designed, synthesized and characterized by 1H, 13C NMR spectroscopy and HRESI mass spectrometry. The introduction of alkenyl bonds endowed the [2]rotaxane a fascinating ability to react with versatile functional groups such as alkenyl and thiol functional groups. The reversible shuttling movement of the macrocycle between two different recognition sites on the molecular thread can be driven by external acid and base. This kind of rotaxane bearing functional groups provides a powerful platform for preparing stimuli-responsive polymers.

9-Silyl(-Germyl,-Stannyl) Substituted Derivatives of 1-(9-Fluorenyl)- germatranes. Synthesis, Characterisation, and Crystal Structures

1998 ◽  
Vol 53 (11) ◽  
pp. 1247-1254 ◽  
Author(s):  
Galina S. Zaitseva ◽  
Sergey S. Karlov ◽  
Bettina A. Siggelkow ◽  
Evgeni V. Avtomonov ◽  
Andrei V. Churakov ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Elemental Analyses ◽  
Derivatives Of ◽  
C Nmr

9-Trimethylsilyl- and 9-trimethylgermyl substituted derivatives of 1-(9-fluorenyl)germatranes C13H8(R)Ge(OCH2CH2)3N (1 - 3) (1: R = H; 2: R = Me3Si; 3: R = Me3Ge) were prepared by the reaction of 9-tribromogermyl derivatives of fluorene C13H8(R)GeBr3 (4 - 6) with N(CH2CH2OSnAlk3)3 (7: Alk = Et; 8: Alk = Bu). 1-(9-Trimethylstannyl- 9-fluorenyl)germatrane (14) was synthesised by the reaction o f the germatrane (1) with Me3SnNMe2 . Formulas and structures were established by elemental analyses, (1H, 13C) NMR spectroscopy and mass spectrometry; crystal structures of 2 and 14 are reported.

Synthesis, spectroscopic characterization, and structural studies of organogermanium tri- and monothiocarbonates. Crystal structures of Me2Ge[S2CSEt]2, Ph3Ge[SCO2Me], Ph3Ge[SCO2(i-Pr)], and Ph2Ge[SCO2Me]2

1998 ◽  
Vol 76 (3) ◽  
pp. 319-334 ◽  
Author(s):  
John E Drake ◽  
Jincai Yang
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Sodium Salt ◽  
Variable Temperature ◽  
Spectroscopic Characterization ◽  
Structural Studies ◽  
Cell Parameters ◽  
Derivatives Of ◽  
C Nmr

Two series of S-alkyl trithiocarbonate derivatives of imethylgermane, Me2Ge[S2CSR]2, and halodiphenylgermane, Ph2GeX[S2CSR], where R = Me, i-Pr, n-Pr, n-Bu and X = Cl, Br, and three series of O-alkyl monothiocarbonate derivatives of triphenylgermane, Ph3Ge[SCO2R], diphenylgermane, Ph2Ge[SCO2R], and trimethylgermane, me3Ge[SCO2R], where R = Me, i-Pr, and n-Pr, have been prepared in 73-92% yields by the reaction of the potassium or sodium salt of the appropriate tri- or monothiocarbonic acid with dichlorodimethyl-, chlorotriphenyl-, dichlorodiphenyl-, and chlorotrimethylgermane. The compounds were principally characterized by infrared, Raman, and 1H and 13C NMR spectroscopy, including some variable temperature studies, as well as by mass spectrometry. Me2Ge[S2CSEt]2, 1: P21/m (No. 11) with cell parameters a = 6.647(4) Å, b = 7.423(2) Å, c = 16.290(4) Å, β = 91.07(3)°, V = 803.6(4) Å3, Z = 2, R = 0.0484,Rw = 0.0485. Ph3Ge[SCO2Me],13: P1bar (No. 2) with cell parameters a = 9.970(4) Å, b = 10.660(3) Å, c = 9.853(2) Å, α = 101.78(2)°, β = 109.98(2)°, γ = 89.76(3)°, V = 961.0(5) Å3, Z = 2, R = 0.0534, Rw = 0.0451. Ph3Ge[SCO2(i-Pr)], 14: P 1bar (No. 2) with cell parameters a = 14.386(7) Å, b = 18.598(6) Å, c = 9.223(3) Å, α = 102.85(3)°, β = 94.58(3)°, γ = 108.13(3)°, V = 2256(1) Å3, Z = 2, R = 0.0545, Rw = 0.0552. Ph2Ge[SCO2Me]2, 16: Cc, (No. 9) with cell parameters a = 11.790(4) Å, b = 13.696(5) Å, c = 23.232(6) Å, β = 92.26(3)°, V = 3748(2) Å3, Z = 8, R = 0.0563, Rw = 0.0512. The immediate environment about Ge is that of tetrahedral but the orientations of the thiocarbonate groups display interesting features.Key words: structure, germanium, phenyl, methyl, thiocarbonates.

Synthesis and Single Crystal X-Ray Structure of Ethyl 2-(1,3-Benzoxazol- 2-yl)-5-oxo-3-(4-toluidino)-2,5-dihydro-4-isoxazolecarboxylate

2007 ◽  
Vol 62 (5) ◽  
pp. 705-710 ◽  
Author(s):  
Ali Souldozi ◽  
Jabbar Khalafy ◽  
Ahmad Poursattar Marjani ◽  
Katarzyna Ślepokura ◽  
Tadeusz Lis ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Structure Determination ◽  
Single Crystal Structure ◽  
Crystal Structure Determination ◽  
X Ray ◽  
C Nmr

Abstract Ethyl 5-oxo-3-(4-toluidino)-2,5-dihydro-4-isoxazolecarboxylate was prepared from the reaction of diethyl 2-(4-toluidinocarbothioyl)malonate with hydroxylamine. Its reaction with 2- chlorobenzoxazole gave the corresponding N-substituted isoxazolone. The structure of the final product 4 was confirmed by IR, 1H and 13C NMR spectroscopy and mass spectrometry, and by X-ray single crystal structure determination.

scholarly journals Synthesis And Single Crystal X-Ray Structure Of 2-(1,3,4-Oxadiazol- 2-yl)Aniline

2007 ◽  
Vol 62 (6) ◽  
pp. 835-840 ◽  
Author(s):  
Ali Souldozi ◽  
Katarzyna Ślepokura ◽  
Tadeusz Lis ◽  
Ali Ramazani
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Single Crystal ◽  
Structure Determination ◽  
High Yield ◽  
Aminobenzoic Acid ◽  
Aromatic Rings ◽  
X Ray ◽  
C Nmr

Reaction of 2-aminobenzoic acid with (N-isocyanimino)triphenylphosphorane proceeds smoothly at r. t. to afford 2-(1,3,4-oxadiazol-2-yl)aniline in high yield. The structure of this compound was confirmed by IR, 1H, and 13C NMR spectroscopy, mass spectrometry, and single crystal X-ray structure determination. The X-ray structural analysis of the product indicated that its aromatic rings are approximately co-planar

Syntheses and Characterization of 1-Haloazagermatranes

2001 ◽  
Vol 56 (2) ◽  
pp. 137-140 ◽  
Author(s):  
Pavel L. Shutov ◽  
Sergey S. Karlov ◽  
Jörg Lorberth ◽  
Galina S. Zaitseva
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Molecular Composition ◽  
High Yield ◽  
Elemental Analyses ◽  
New Compounds ◽  
C Nmr

Abstract Germanium, Azagermatranes The reaction of tris(dimethylamino)halogermanes, (Me2N)3GeHal (7, Hal = Cl; 8 , Hal = Br), with tris(2-aminoethyl)amines, N(CH2CH2NHR)3 (5, R = H; 6 , R = Me), yield l-halo-N,N',N"-azagermatranes (1, X = Cl, R = H; 2, X = Br, R = H; 3, X = Cl, R = Me; 4, X = Br, R = Me). Treatment of 4 with n-butyllithium affords l-n-butyl-N,N',N"-trimethylazagermatrane (14) in high yield. Reactions of n-BuLi with 7 or (Me2N)4Ge (13) lead to the formation of (Me2N)3Ge-n-Bu (15). On treatment of 15 with 5 the 1 -n-butylazagermatrane 16 was obtained. The molecular composition and the structures of all new compounds were established by elemental analyses, 1H and 13C NMR spectroscopy and mass spectrometry.

Chemistry of the 1,3,5-Triaza-2-phosphorin-4,6-diones, Part XII*. Synthesis and Characterization of 2-PhenyI-2-(p-tolylthio)-1,3,5- trimethyI-1,3,5-triaza-4,6-dione-2-phosphorinonium Salts

1996 ◽  
Vol 51 (10) ◽  
pp. 1494-1500 ◽  
Author(s):  
Vasily A . Pinchuk ◽  
Ion Neda ◽  
Christian Müller ◽  
Holger Thönnessen ◽  
Peter G. Jones ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
New Products ◽  
Synthesis And Characterization ◽  
Tetrahedral Geometry ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Weak Hydrogen Bonds ◽  
C Nmr

The reaction of 1,5-bis(trimethylsilyl)-1,3.5-trimethylbiuret (1) with p-tolylsulfenyl chloride (2) furnished l-(p-tolylthio)-5-trimethylsilyl-1,3,5-trimethylbiuret (3). In the reaction of 3 with phenyldichlorophosphine, 2-phenyl-2-(p-tolylthio)-1,3,5-trimethyl-1,3,5-triaza-4,6-dione- 2-phosphorinonium chloride (4) was formed. The same product was obtained from the reaction of 2-phenyl-1,3,5-trimethyl-1,3,5-triaza-2λ3- phosphorin-4,6-dione (6) with p-tolylsulfenyl chloride (2). Compound 4 was isolated and characterized in the form of the hexachloroantimonate (4a). The spirophosphorane 2-phenyl-1,3,5-trimethyl-1,3,5-triaza-7,10-dioxa-8,9- perchlorobenzo-2λ5-phosphaspiro-[4.5]decan-4,6-dione (7) was prepared by the reaction of 4 with tetrachloroorthobenzoquinone. The new products were characterized by 1H - and 13C NMR spectroscopy, elemental analysis, 31P NMR spectroscopy in the case of 4a. 6 and 7, and mass spectrometry (4a). Single-crystal X-ray structural analyses of compounds 4a and 7 were conducted. The phosphorus atom of 4a has the expected tetrahedral geometry, with a rather short P-S bond of 204.9(2) pm. In 7 the geometry at phosphorus is almost ideal trigonal bipyramidal. Weak hydrogen bonds are formed from a C (:O) group to deuterochloroform of solvation.

scholarly journals Some New Heterocyclisations Based on N-(2,2-dichloro-1-isothiocyanatoethyl)benzamide Derivatives

2019 ◽  
Vol 27 (1) ◽  
pp. 65-72
Author(s):  
Ihor O. Pokotylo ◽  
Pavlo V. Zadorozhnii ◽  
Vadym V. Kiselev ◽  
Oxana V. Okhtina ◽  
Aleksandr V. Kharchenko
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Mass Spectrometry Data ◽  
Benzamide Derivatives ◽  
C Nmr

Abstract Based on the readily available N-(2,2-dichloro-1-(2-(4-methylbenzoyl)-hydrazine-1-carbothioamido)ethyl)benzamide, the corresponding N-(2,2-dichloro-1-((5-(p-tolyl)-1,3,4-oxadiazol-2-yl)amino)ethyl)benzamide and 5-(p-tolyl)-1,3,4-thiadiazol-2-amine were obtained. The products were received in acceptable yields and were isolated from the reaction mixture without any particular difficulty. The structure of the compounds obtained was confirmed by 1H, 13C NMR spectroscopy and mass spectrometry data.

Design, synthesis and crystallographic study of novel indole-based cyano derivatives as key building blocks for heteropolycyclic compounds of major complexity

2017 ◽  
Vol 73 (12) ◽  
pp. 1040-1049 ◽  
Author(s):  
Andrés C. García ◽  
Rodrigo Abonía ◽  
Luz M. Jaramillo-Gómez ◽  
Justo Cobo ◽  
Christopher Glidewell
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Ambient Temperature ◽  
Elemental Analysis ◽  
Building Blocks ◽  
Reaction Sequence ◽  
Design Synthesis ◽  
Crystallographic Study ◽  
Triclinic Form ◽  
C Nmr

A four-stage reaction sequence has been designed and developed for the synthesis of highly functionalized enolate esters as key building blocks for the synthesis of novel heteropolycyclic compounds of potential pharmaceutical value. The sequence starts with simple commercially available indoles and proceeds via 3-(indol-3-yl)-3-oxopropanenitriles, which react with 2-bromobenzaldehyde to form the corresponding chalcones; these are readily reduced to dihydrochalcones, which are in turn acylated to form the enolate esters. The compounds in this sequence have been characterized by IR and 1H and 13C NMR spectroscopy, by mass spectrometry and by elemental analysis. The molecular and supramolecular structures are reported for representative examples, namely (E)-3-(2-bromophenyl)-2-(1-methyl-1H-indole-3-carbonyl)acrylonitrile, C19H13BrN2O, (Ib), (2RS)-2-(2-bromobenzyl)-3-(1-methyl-1H-indol-3-yl)-3-oxopropanenitrile, C19H15BrN2O, (IIb), and (2RS)-3-(1-benzyl-1H-indol-3-yl)-2-(2-bromobenzyl)-3-oxopropanenitrile, C25H19BrN2O, (IIc), the latter two of which crystallize with Z′ = 2, and (E)-1-(1-acetyl-1H-indol-3-yl)-3-(2-bromophenyl)-2-cyanoprop-1-en-1-yl acetate, C22H17BrN2O, (III), and (E)-1-(1-benzyl-1H-indol-3-yl)-3-(2-bromophenyl)-2-cyanoprop-1-en-1-yl benzoate, C32H23BrN2O, (IV). The structure of the related chalcone (E)-2-benzoyl-3-(2-bromophenyl)prop-2-enenitrile, (V), has been redetermined at 100 K, where it is monoclinic, as opposed to the triclinic form reported at ambient temperature.

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