Reaction of CO2 and CS2 with Aniline Catalyzed by AlCl3 under Mild Condition

2013 ◽  
Vol 575-576 ◽  
pp. 531-534 ◽  
Author(s):  
Hong Xing Xu ◽  
Xin Hua Yuan

The reactions of aniline with CO2and CS2were investigated in the presence of sublimed AlCl3under the mild conditions (room temperature and ambient atmosphere). Reasonable mechanism, electrophilic substitution of carbonium and nitronium, was also provided according to GC/MS analysis of the reaction products. The resulting N,N-diphenylurea (DPU, high selectivity of 92.5mol%) and N,N-diphenyl thiourea (DPTU, high yield and selectivity of 80.1mol% and 99.7mol%, respectively) were purified by recrystallizing from ethanol and identified by melting point, element analysis, GC/MS, FTIR, UV and1H NMR data.

2014 ◽  
Vol 525 ◽  
pp. 93-96
Author(s):  
Wei Shi ◽  
Ji Ming Zhang ◽  
Jian Hua Zhou ◽  
Jian Hua Zhou ◽  
Song Song Ding

Herein we describle a facile synthesis of sulphonic acid oxime esters in acetonitrile from the corresponding sulphonic acids and oximes catalyzed by the environmental friendly 2-(1H-benzotriazole-1-yl)-1,1,3,3-tetramethyluronium tetrafluoroborate (TBTU) in the presence of triethylamine (TEA) under mild conditions. The present approach offers the advantages of a clean reaction, simple methodology, employing readily available catalyst, short reaction duration, high selectivity and high yield.


2005 ◽  
Vol 3 (3-4) ◽  
pp. 289-297 ◽  
Author(s):  
A. K. Srivastava ◽  
O. P. Pandey ◽  
S. K. Sengupta

The reactions of bis(cyclopentadienyl)titanium(IV) dichloride with Schiff bases derived by condensing 2- amino-5-phenyl-1,3,4-thiadiazole with benzaldehyde (SPT), 4-nitrobenzaldehyde (SNT), 4-methoxybenzaldehyde (SMT), 2-hydroxybenzaldehyde (SSTH) or 2-hydroxyacetophenone (SATH) have been studied in refluxing tetrahydrofuran and complexes of types [Cp2TiCl(SB)]Cl (SB= SPT, SNT or SMT) and [Cp2Ti(SB')]Cl (SB'H= SSTH or SATH) have been isolated. Tentative structural conclusions are drawn for these reaction products based upon elemental analyses, electrical conductance, magnetic moment and spectral (UV-vis, IR and1H NMR) data. Studies were conducted to assess the growth-inhibiting potential of the complexes synthesized, and the ligands, against various fungal and bacterial strains.


1993 ◽  
Vol 47 (3) ◽  
pp. 357-359 ◽  
Author(s):  
A. L. Cholli ◽  
M. L. Lau

High-resolution 1H NMR has been used to study the molecular dynamics of the piperidine derivative. Detailed analysis of variable temperature NMR data allowed the identification of the origin of two sets of methyl resonance peaks with unequal intensities in the room-temperature proton NMR spectrum of the compound.


2001 ◽  
Vol 665 ◽  
Author(s):  
Yuning Li ◽  
George Vamvounis ◽  
Steven Holdcroft

ABSTRACTThe electrophilic substitution of regioregular poly(3-hexylthiophene) (P3HT) at the 4- position was investigated to produce structurally well defined 3,4-disubstituted poly(thiophene)s. When P3HT was treated with N-bromosuccinimide (NBS) in chloroform at 25 to 50 °C, the 4-hydrogen atom in P3HT is completely substituted by bromine, as indicated by the 1H NMR, 13C NMR and elemental analysis. Similarly, the chlorinated product was obtained using N- chlorosuccinimide (NCS) at room temperature. However, only 85% of the 4-hydrogen atoms were replaced by chlorine and ∼15% of the α-hydrogen atoms on the hexyl side chain were chlorinated. P3HT readily reacts with fuming nitric acid in chloroform at 0 °C to generate a nitrated product with almost 100% substitution at the 4-position. Our preliminary study on the futher functionalizaton of these polymers was conducted on the brominated product. Our results showed that the bromine atom in this polymer could be further substituted with other groups.


1983 ◽  
Vol 38 (4) ◽  
pp. 497-500 ◽  
Author(s):  
E. L. Michelotti ◽  
E. L. Sanchez

Abstract A stereospecific synthesis of 4,8-dimethylspiro(4,5)-deca-7-ene-1,6-dione from 4,7-dimethylcoumarine in high yield is reported. The configuration of this product is established according to its 1H NMR and 13C NMR data.


1979 ◽  
Vol 57 (23) ◽  
pp. 3107-3112 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter

Ni(NO)I reacts readily with pyrazolyl gallate ligands Na+L− (where L = MeGa(N2C3H3)3, MeGa(N2C5H7)3, and [Me2Ga(N2C5H7)(OCH2CH2NMe2)]) to yield four-coordinate nickel nitrosyl complexes, LNi(NO). In addition, the compound [Me2Ga(N2-C5H7)(OCH2CH2 NMe2)]Ni(N2C5H7)2Ni(NO) has been isolated from one reaction sequence. 1H nmr data show [Me2Ga(N2C5H7)(OCH2CH2NMe2)]Ni(NO) to be stereochemically non-rigid at room temperature in solution. Crystals of [dimethyl(N,N-dimethylethanol-amino)(3,5-dimethylpyrazolyl)gallato(N(2),N(3),O)] nitrosylnickel(I) are monoclinic, a = 9.119(1), b = 13.900(2), c = 14.284(2) Å, β = 107.96(1)°, Z = 4, space group P21/c. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix leastsquares procedures to R = 0.025 and Rw = 0.032 for 1828 reflections with I ≥ 3σ(I). The coordination about the nickel atom is severely distorted tetrahedral with angles at nickel ranging from 84.4(1) to 133.5(1)°. The nitrosyl group is coordinated in a non-linear fashion with Ni—N—O = 162.3(4)°, Ni—N = 1.632(4) and N—O = 1.147(4) Å. Other important bond lengths (corrected for libration) are: Ni—O, 2.045(2), Ni—N(pyrazolyl), 1.989(3), Ni—N(amino), 2.071(3), Ga—O, 1.922(2), Ga—N, 1.998(3), and Ga—C, two at 1.971(6) Å.


2020 ◽  
Vol 44 (21) ◽  
pp. 8710-8717
Author(s):  
André L. D. Lima ◽  
Humberto V. Fajardo ◽  
André E. Nogueira ◽  
Márcio C. Pereira ◽  
Luiz C. A. Oliveira ◽  
...  

Nb-peroxo@iron oxides show high selectivity and activity in aniline conversion to azoxybenzene.


2020 ◽  
Author(s):  
Subham Mahapatra ◽  
Cristian P. Woroch ◽  
Todd W. Butler ◽  
Sabrina N. Carneiro ◽  
Sabrina C. Kwan ◽  
...  

<p><br></p> <p>A method to activate sulfamoyl fluorides, fluorosulfates, and sulfonyl fluorides with calcium triflimide, and DABCO for SuFEx with amines is described. The reaction was applied to a diverse set of sulfamides, sulfamates, and sulfonamides at room temperature under mild conditions. Additionally, we highlight the application of this transformation to parallel medicinal chemistry to generate a broad array of nitrogen-based S(VI) compounds. </p>


2020 ◽  
Author(s):  
Subham Mahapatra ◽  
Cristian P. Woroch ◽  
Todd W. Butler ◽  
Sabrina N. Carneiro ◽  
Sabrina C. Kwan ◽  
...  

<p><br></p> <p>A method to activate sulfamoyl fluorides, fluorosulfates, and sulfonyl fluorides with calcium triflimide, and DABCO for SuFEx with amines is described. The reaction was applied to a diverse set of sulfamides, sulfamates, and sulfonamides at room temperature under mild conditions. Additionally, we highlight the application of this transformation to parallel medicinal chemistry to generate a broad array of nitrogen-based S(VI) compounds. </p>


2020 ◽  
Vol 17 (8) ◽  
pp. 654-660
Author(s):  
Shermineh Sadat Ghalehbandi ◽  
Dadkhoda Ghazanfari ◽  
Sayed Ali Ahmadi ◽  
Enayatollah Sheikhhosseini

Introduction: We developed a simple, fast and new method for the Fries rearrangement of aryl esters. Materials and Methods: 4-Hydroxy pyridinium triflate functionalized silica is a very efficient, reusable and economically available catalyst for the Fries rearrangement in solvent-free condition and under microwave irradiation. Results and Discussion: Also, a notable selectivity was observed in the presence of 4-hydroxy pyridinium triflate functionalized silica. Conclusion: Selectivity, shorter reaction time, high yield, and easy work-up are advantages of this synthetic method.


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