Search results for "ethylamine"
showing 10 items of 230 documents
Ortho-Metalated Primary Amines. 6.1 The First Synthesis of Six-Membered Palladacycles from Primary Amines Containing Electron-Withdrawing Substituent…
2003
When H 2 N(CH 2 ) 2 C 6 H 4 OMe-4 (RNH 2 ) and Pd(OAc) 2 are reacted in a 2:1 molar ratio, the complex [Pd(OAC) 2 (NH 2 R) 2 ] (1) is obtained. Complex 1 reacts with 1 equiv of Pd(OAc) 2 to give the dinuclear complex [Pd(OAc)(μ-OAc)(NH 2 R)] 2 (2). When complex 2 is heated in acetonitrile at 80 °C, the ortho-metalated complex [Pd{C 6 H 3 (CH 2 ) 2 NH 2 -2-OMe-5-κ 2 C,N}(μ-OAc)] 2 (3a) is obtained. Complex 3a is also prepared by refluxing RNH 2 and Pd(OAc) 2 in a 1:1 molar ratio in acetonitrile. Complex 3a reacts with NaBr or LiCl to afford the complexes [Pd{C 6 H 3 (CH 2 ) 2 NH 2 -2-OMe-5-κ 2 C,N}(μ-X)]2 (X = Cl (3b), Br (3c)). PPh 3 splits the acetate or halide bridge in complex 3a or 3b t…
Synthesis and in vitro antileukemic activity of new 4-triazenopyrazole derivatives
2003
Several new 4-(3,3-dimethyltriazeno)-5-benzamidopyrazole derivatives were prepared by reacting 4-diazo-5-benzamidopyrazole derivatives with dimethylamine. The compounds were tested at 10 microM for their vitro antileukemic activity against K562 (Human chronic myelogenous leukemia) and Raji (human Burkitt limphoma ) cell lines. Dacarbazine and methotrexate were used for comparative purpose. The 3-methyl-4-(3,3-dimethyltriazeno)-5-(substituted benzamido)pyrazoles, bearing the pyrazole nucleus free at 1 position, resulted more active than the 1-(substituted phenyl)-3-methyl-4-(3,3-dimethyltriazeno)-5-benzamidopyrazoles. Dacarbazine at 10 microM showed no activity in the above tests. The observ…
Über polygermane
1986
Abstract The germylene Ph2Ge of Ph2GeHCl and Net3 inserts in excess Ph2GeHCl and forms polygermanes Cl(Ph2Ge)nH. This one-pot reaction and subsequent chlorination to Cl(Ph2Ge)nCl has been optimized. Increasing amounts of NEt3 step up the yields of higher polygermanes. The 13C NMR phenyl signals for C(ipso) shift to low field with increasing chain length. The crystal structures of Cl(Ph2Ge)3,4Cl (R = 0.072 and 0.087) have been determined. The position of Cl(Ph2Ge)4Cl is split off by disorder (main molecule 82%, side molecule 18%). Two crystallographically different molecules of the trigermane are present; the ClGe3Cl chain contains anti-gauche and gauche-gauche conformation respectively (d…
On the reaction of 3-bromo-2-nitrobenzo[b]thiophene with some ortho-substituted anilines: an analysis of the products of reaction and of their NMR an…
2003
Abstract The title reaction, carried out in DMF in the presence of triethylamine or potassium carbonate, has furnished the ‘expected’ 3-amino-2-nitrobenzo[ b ]thiophenes 2 o together with the ‘unexpected’ 2-amino-3-nitrobenzo[ b ]thiophenes 3 o , thus recalling the situation observed with other weak nucleophiles in the presence of non-nucleophilic bases. The effects (electronic as well as steric) of the ortho -substituent (OH, NH 2 , OMe, Me, Et, F, Cl and Br) on the course of the reaction have been investigated, determining their influence on yields and product ratios ( 2 o / 3 o ). An analysis of 13 C NMR and MS spectra of 2 o and 3 o has been carried out. Ab initio computations on 2 o f …
Zinc-salophen complexes as selective receptors for tertiary amines
2007
Zinc-salophen compounds 1-3 incorporating in the given order 1,2-diaminobenzene, 2,3-diaminonaphthalene, and 9,10-diaminophenantrene moieties were synthesised. Their binding properties toward a series of tertiary amines were assessed by UV-Vis and fluorescence spectroscopy in chloroform solution. Unprecedented selectivities of quinuclidine vs. triethylamine higher than 105 were recorded, thereby revealing the dramatic influence of steric effects on axial coordination of tertiary amines. X-Ray diffraction analyses showed that in the solid state compound 2 is dimeric, but its 1 : 1 quinuclidine complex is monomeric. Strong indications were obtained that both free receptors and their amine add…
Mononuclear rearrangement of heterocycles in zwitterionic micelles of amine oxide surfactants.
2012
Abstract Rate constants for the mononuclear rearrangement (MRH) of Z -phenylhydrazones of some 5-substituted-3-benzoyl-1,2,4-oxadiazoles in water have been measured in the presence of zwitterionic micelles. The use of micellized N -tetradecyl- N , N -dimethylamineoxide (C 14 DMAO) as the reaction medium allowed to solubilize the otherwise water-insoluble oxadiazoles. Micellar rate effects were analyzed by using a simple pseudo-phase model and compared with those obtained in non-ionic micelles (Triton X-100). Evidence that both the rate of the rearrangement reaction and the binding of the substrates to the micelles are mainly governed by substrate hydrophobicity is obtained. The disagreement…
Preparation and reactions of 1-methylpyrid-6-one-2-yl compounds of palladium(II) and platinum(II)
1984
Abstract The compounds trans -[MCl{(1-Me)C 5 H 3 (6-O)N- C 2 }(L) 2 ] (M = Pd, Pt; L = PPh 3 , PMe 2 Ph), can be prepared from the reaction of the corresponding 1-methyl-6-chloro-2-pyridylium cationic complexes, trans -[MCl{(1-Me)C 5 H 3 (6-Cl)N- C 2 }(L) 2 ]ClO 4 , with a mixture of acetic acid, ethanol, and triethylamine in the molar ratio M/MeCO 2 H/EtOH/NEt 3 of 1/3/3/4. The rate is slow compared to that of the 1-methyl-2-chloropyridinium cation under similar conditions, and is markedly affected by the steric and electronic effects of the trans -MCl(L) 2 unit. The novel 1-methylpyrid-6-one-2-yl derivatives have been characterized by conventional spectroscopic techniques and by reactions…
INSERTION OF ISOCYANIDES INTO THE PALLADIUM CARBON BOND OF C-2-PALLADATED HETEROCYCLES - SYNTHESIS OF TRANS-[PDCL(C(RN)=NR) (PPH3)2] COMPLEXES (RN = …
1985
The titles complexes trans-[PdCl{C(RN)NR}(PPh3)2] (RN = 2-pyridyl (2-py), R = p-C6H4OMe, Me; RN = 2-pyrazyl (2-pyz), R = p-C6H4OMe) can be prepared by reaction of the N-protonated compounds, cis-[PdCl2(RNH)(PPh3] (RNH = 2-pyridylium (2-pyH) or 2-pyrazylium (2-pyzH) group), with PPh3, followed by addition of the isocyanide CNR and deprotonation with triethylamine, in a molar ratio Pd/PPh3/CNR/NEt3 of 1/1/1/1.1. The reaction sequence involves the successive formation of the cationic intermediates trans-[PdCl(RNH)(PPh3)2]+, trans-[Pd(RNH)(CNR)(PPh3)2]2+ and trans-[Pd(RN)(CNR)(PPh3)2]+, which were isolated and characterized as perchlorate salts for RN = 2-pyridyl. In the final step the coordin…
Ligand substitution reactions of the [ReX6]2− (X=Cl, Br) anions. Synthesis and crystal structure of novel oxalato complexes of rhenium(IV)
2006
Abstract The reaction of K2[ReX6] (X = Cl, Br) with oxalic acid and triethylamine in dimethylformamide solution yields the substituted complexes [ReX4(ox)]2− and cis-[ReX2(ox)2]2−, which can be obtained separately depending on the amount of added amine. The crystal structures of (PPh4)2[ReBr4(ox)], cis-(PPh4)2[ReBr2(ox)2] and cis-(AsPh4)2[ReCl2(ox)2] have been determined by single-crystal X-ray diffraction. The anionic complexes are octahedral with only slight distortions. The direct isolation of the pure complexes as well as the formation of only the cis isomers – without the presence of trans isomers and/or [Re(ox)3]2− – is probably due to the kinetic inertness of Re(IV)–X bonds, which in…
Preparation of 2-amino-5-methyl-7H-1,3,4-thiadiazolo[3,2-α]pyrimidin-7-ones
2005
2-Amino substituted 7H-1,3,4-thiadiazolo[3,2-α]pyrimidin-7-ones 11a-e were prepared by the reaction of 2-bromo-5-amino-1,3,4-thiadiazole (1b) and diketene (8), subsequent cyclocondensation (9b 3b) and displacement of the bromo substituents by the reaction with primary or secondary amines (3b 11a-e). The hydrogen atom 6-H in the heterobicycle 3b is replaced by a Cl or Br atom in the transformation of 3b 14a,b. The 2-bromo-6-chloro compound 14a reacts chemoselectively in the 2-position with dimethylamine (14a 15). The structure elucidations are based on one- and two-dimensional NMR techniques including a heteronuclear NOE measurement.