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1.
Carlos Camacho-Camacho Maria E. Castillo-Ramos Aurora Vásquez-Badillo Angelina Flores-Parra Rosalinda Contreras 《Journal of organometallic chemistry》2010,695(6):833-9863
The syntheses of [bis(3,5-di-tert-butyl-2-hydroxy-2-phenyl)amine]diphenyltin (1) and [bis(3,5-di-tert-butyl-2-hydroxy-2-phenyl)amine]dichloro-phenyl-stannate (2) by template reactions using 3,5-di-tert-butylcatechol, aqueous ammonia and SnPh2Cl2 are reported. We also report the syntheses of compounds 2, [bis(3,5-di-tert-butyl-2-hydroxy-2-phenyl)amine]trichloro-stannate (4), [bis(3,5-di-tert-butyl-2-hydroxy-2-phenyl)methylamine]chloro-methyltin (5), and [bis(3,5-di-tert-butyl-2-hydroxy-2-phenyl)-n-butylamine]n-butyl-chlorotin (6) and [bis(3,5-di-tert-butyl-2-hydroxy-2-phenyl)amine]n-butyl-dichloro-stannate (7), performed by transmetallation reactions of the octahedral zinc coordination compound Zn[3,5-di-tert-butyl-1,2-quinone-(3,5-di-tert-butyl-2-hydroxy-1-phenyl)imine]2 (3) with SnPhCl3 or SnPh2Cl2, SnCl4, SnMe2Cl2, Sn(nBu)2Cl2 and Sn(nBu)Cl3, respectively. The X-ray diffraction structures of compounds 1, 2, 4 and 6 are reported. The transmetallation reactions with Sn(alkyl)2Cl2 afforded pentacoordinated tin compounds, where an alkyl group migrated from tin to nitrogen, while similar reactions with Sn-Ph compounds did not present any phenyl group migration. 相似文献
2.
Marisol Güizado-Rodríguez Víctor M. Jiménez-Pérez Jesús E. Hernández-Rivera J.M. Domínguez Rosalinda Contreras Raúl Quijada 《Polyhedron》2007
New non-metallocene polymerization catalysts derived from 1,2-bis(3,5-di-tert-butyl-2-hydroxiphenyl)oxamide (L) and transition metals (Ti, Zr, Hf) were synthesized and tested for ethylene polymerization reactions. The syntheses were carried out from various bases and solvents (triethylamine/toluene, NaH/THF and NaOH/methanol). The zirconium compound (5) showed the highest catalytic activity (the polyethylene molecular weight was 98,000 Da) and polydispersity index (1.8–2.0) when n-heptane was used as solvent. In terms of Tm and crystallinity, this catalyst produced the highest density linear polyethylene. 相似文献
3.
Noemí Andrade-Lpez Rocío Cartas-Rosado Efrn García-Baz Rosalinda Contreras Hugo Tlahuext 《Heteroatom Chemistry》1998,9(4):399-409
The syntheses and structure determinations of a series of boron heterocycles derived from 2-guanidinobenzimidazole 1 are reported. Structures of new compounds, 2-guanidino-1-methyl-benzimidazole 2, diphenyl-(2-guanidinobenzimidazole-N,N′)-borate 3, diphenyl-(2-guanidino-1-methyl-benzimidazole-N,N′)borate 4, hydroxy-phenyl-(2-guanidino-benzimidazole-N,N′)borate 5, hydroxy-phenyl-(2-guanidino-1-methyl-benzimidazole-N,N′)borate 6,methoxy-phenyl-(2-guanidinobenzimidazole-N,N′)borate 7, isopropoxy-phenyl-(2-guanidinobenzimidazole-N,N′)borate 8, acetoxy-phenyl-(2-guanidinobenzimidazole-N,N′)borate 9, methoxy-phenyl-(2-guanidino-1-methyl-benzimidazole-N,N′)borate 10, dihy-droxy-(2-guanidino-1-methyl-benzimidazole-N,N′)borate 16, difluoro-(2-guanidinobenzimidazole-N,N′)borate, 17, dihydroxy-(2-guanidino-1-benzimidazole-N,N′)borate potassium salt 19, diphenyl-(2-guanidinium-10H-benzimidazole-N,N′)borate hydro-chloride 20, methoxy-phenyl-(2-guanidinobenzimidazole-N,N′)borate hydrochloride 21, and N10-borane-(diphenyl-2-guanidinobenzimidazole-N,N′)borate 22, were determined based on 1H, 13C, 15N, and 11B spectroscopy. The X-ray diffraction structures of 3–7, 19, and 20 were obtained. The formation of N3-borane adducts 11 and 12 derived from compounds 1 and 2, respectively, and the dihydride-(2-guanidinobenzimidazole-N,N′)borate 13 and dihydride-(2-guanidino-1-methyl-benzimidazole-N,N′)borate 14 were observed by 11B NMR. The results show that 2-guanidinobenzimidazole gives stable borate heterocycles with a delocalized π electronic system. A dynamic exchange of N–H protons was observed with preferred protonation at N-12. The new heterocycles are protonated at N-10 by acidic substances to give pyridinium-type heterocycles or can lose a proton to give iminium salts. © 1998 John Wiley & Sons, Inc. Heteroatom Chem 9:399–409, 1998 相似文献
4.
Raúl Salas-Coronado Raúl Colorado-Peralta Rosalinda Contreras 《Journal of organometallic chemistry》2009,694(5):616-622
N-Benzyl-4-hydroxy-butyramide (1), 4-hydroxy-N-[(R)-1-phenyl-ethyl]-butyramide (2), and (R)-4-hydroxy-2-methyl-N-[(R)-1-phenyl-ethyl]-butyramide (3a) were used to prepare new diphenylboron and triphenyltinoxy compounds: diphenylborinic acid 3-benzylcarbamoyl-propyl ester (4), diphenylborinic acid 3-[(R)-1-phenyl-ethylcarbamoyl]-propyl ester (5) and diphenylborinic acid (R)-3-[(R)-1-phenyl-ethylcarbamoyl]-butyl ester (6), N-benzyl-4-triphenyltinoxy-butyramide (7), 4-triphenyltinoxy-N-[(R)-1-phenyl-ethyl]-butyramide (8), and (R)-4-triphenyltinoxy-2-methyl-N-[(R)-1-phenyl-ethyl]-butyramide (9). The X-ray diffraction analysis of a crystalline structure of the new γ-hydroxyamide 3a is reported, as well as that of the first example of a crystalline structure where a diphenylborinic ester forms a seven membered chelate, by a carbonyl coordination to boron (4). Structural studies of tin and boron esters were performed by NMR. The CO internal coordination to tin atoms, affording seven membered rings, was observed by 119Sn NMR experiments at low temperature. 相似文献
5.
Adriana Esparza-Ruiz Heinrich Nöth Rosalinda Contreras 《Journal of organometallic chemistry》2009,694(23):3814-2098
The syntheses and structural analyses of a series of boron heterocycles derived from 2-(1H-benzimidazol-2-yl)-phenylamine (1), 2-(1H-benzimidazol-2-yl)-phenol (2), 2-(1H-benzimidazol-2-yl)-benzenedisulfide (3), 2-[3-(1,1,1,3,-tetramethyl-butyl)-phenyl]-2H-benzotriazole (4), 2-[3,5-bis-(1-methyl-1-phenylethyl)-phenyl]-2H-benzotriazole (5) and (C6H5)2BOH or BF3·OEt2 are reported. The new boron compounds: diphenyl-[2-(1H-benzimidazol-2-yl-κN)-phenylamide-κN]-boron (6), diphenyl-[2-(1H-benzimidazol-2-yl-κN)-phenolate-κO]-boron (7), diphenyl-[2-(1H-benzimidazol-2-yl-κN)-benzenethiolate-κS]-boron (8), diphenyl-[2-(2H-benzotriazol-2-yl-κN)-4-(1,1,3,3-tetramethyl-butyl)-phenolate-κO]-boron (9), diphenyl-[2-(2H-benzotriazol-2-yl-κN)-4,6-(1-methyl-1-phenylethyl)-phenolate-κO]-boron (10), difluoro-[2-(1H-benzimidazol-2-yl-κN)-phenolate-κO]-boron (11), difluoro-[2-(2H-benzotriazol-2-yl-κN)-4-(1,1,3,3-tetramethylbutyl)-phenolate-κO]-boron (12) and difluoro-[2-(2H-benzotriazol-2-yl-κN)-4,6-(1-methyl-1-phenylethyl)-phenolate-κO]-boron (13) have four fused rings, with boron included in a six-membered ring and bound to N, O or S atoms and strongly coordinated by a nitrogen atom from the imidazole or triazole rings. Their structures are zwitterionic, with a negative charge on the boron and a delocalized positive charge on the ligand. Compounds 6-12 were studied by NMR, IR, mass spectrometry, and 6-10 and 12 by X-ray diffraction analyses. 相似文献
6.
Raúl Colorado‐Peralta Cristina A. Lpez‐Rocha Sonia A. Snchez‐Ruiz Rosalinda Contreras Angelina Flores‐Parra 《Heteroatom Chemistry》2011,22(1):59-71
The structure and reactivity of a series of new ethylaminedithiazinanes and bis‐diethylaminedithiazinanes synthesized from formaldehyde, NaSH, and N,N‐dimethyl‐ethylene‐diamine ( 1 ), N‐methyl‐ethylene‐diamine ( 2 ), and N‐ethyl‐ethylene‐diamine ( 3 ) are reported. Compound 1 afforded 2‐([1,3,5]‐dithiazinan‐5‐yl)‐ethylene‐N,N‐dimethyl‐amine ( 4 ). The reaction of 4 with dry CH2Cl2 gave N‐{2‐([1,3,5]dithiazinan‐5‐yl)‐ethylene}‐N‐chloromethyl‐N,N‐dimethyl‐ammonium chloride ( 5 ) in high yield, whereas in wet CH2Cl2 and DMSO provided a mixture of 5 with N‐{2‐([1,3,5]‐dithiazinan‐5‐yl)‐ethylene}‐N,N‐dimethyl‐ammonium hydrochloride ( 6 ).bis‐{2‐([1,3,5]‐Dithiazinan‐5‐yl)‐ethylene‐N‐alkyl‐amino}‐methylene‐disulfides ( 7 ) and ( 8 ) formed by two dithiazinanes linked through the chain (CH2)2 NRCH2 S S CH2 NR (CH2)2‐ ( 7 R = methyl, 8 R = ethyl) reacted with CH2Cl2 giving after neutralization of the hydrolysis products the ethylaminedithiazinanes with different pendant N‐groups [ (CH2)2NMeH2+( 9 ); (CH2)2NEtH2+ ( 10 ); (CH2)2NMeH ( 11 ); (CH2)2NEtH ( 12 ); (CH2)2NMeHBH3 ( 13 ) (CH2)2NEtHBH3 ( 14 ). (CH2)2NMe2BH3 ( 15 ), and (CH2)2NEtMeBH3.( 16 )]. The x‐ray diffraction analyses of compounds 5 , 6 , 9 , and 10 are reported. Variable temperature NMR experiments afforded the Δ G≠ of the ring interconversion of the six‐membered heterocycles 6 , 9 , and 10 . © 2010 Wiley Periodicals, Inc. Heteroatom Chem 22:59–71, 2011; View this article online at wileyonlinelibrary.com . DOI 10.1002/hc.20657 相似文献
7.
Hilda R. Morales Martín Pérez-Juárez Laura Cuéllar Lourdes Mendoza Héctor Fernández Rosalinda Contreras 《合成通讯》2013,43(13):1213-1219
A new procedure for the high-yield N-monoalkylation of primary aromatic and aliphatic amines is described. 相似文献
8.
Gárate-Morales José Luis Reyes-Ortega Yasmi Alvarez-Toledano Cecilio Gutiérrez-Pérez René Ramírez-Rosales Daniel Zamorano-Ulloa Rafael Basurto-Uribe Eduardo Hernández-Díaz Julio Contreras Rosalinda 《Transition Metal Chemistry》2002,27(8):906-917
Six novel pinch-porphyrin complexes [(picdien)(protoporphyrinate dimethyl ester)]copper(II) (7), [(picdien)(mesoporphyrinate dimethyl ester)]copper(II) (8) and [(picdien)(deuteroporphyrinate dimethyl ester)]copper(II) (9), [(picdien)(protoporphyrinate dimethyl ester)]zinc(II) (13), [(picdien)(mesoporphyrinate dimethyl ester)]zinc(II) (14) and [(picdien)(deuteroporphyrinate dimethyl ester)]zinc(II) (15), were prepared from the corresponding free copper(II)-porphyrins (4–6), and zinc(II)-porphyrins (10–12) and picdien (N-(3H-imidazol-4-ylmethyl)-N-{2-[(3H-imidazol-4-ylmethyl)-amino]-ethyl}-ethane-2,3-diamine). Spectroscopic studies show that complexes (7–9) and (13–15) have the pinch-porphyrin type structure previously found in iron(III) complex models of peroxidases. Complexes (7–9), were characterized by u.v.–vis., m.c.d., and e.s.r. spectroscopy. E.s.r. spectra of the copper parent compounds (4–6) at ca. 10–2–10–4 M concentrations were typical of copper(II)-dimers. The addition of the picdien ligand broke up the dimers as detected by e.s.r. Compounds (7–9) are predominantly monomeric at ca. 10–3 M concentration. The presence of picdien in (7–9) distorts the porphyrin internal portion of the plane so as to make these four internal nitrogen atoms, coordinated to copper(II), e.s.r.-distinguishable. MO and ligand field theories were used to characterize and to evaluate the directional covalence parameters of compounds (7–9). A non-fully axial, out-of-the-porphyrin-plane bonding was found for (7–9), similar to the bonding of the pinch-porphyrins-iron(III). However the in-plane distortion produced by the presence of the picdien ligand on copper(II) is significantly larger than in pinch-porphyrin-iron(III). The n.m.r. data show that the porphyrin-zinc(II) is the less strained and has the weakest bonded structure. The coordination number of the pinch-porphyrin with iron(III), copper(II) and zinc(II), is in all cases six. 相似文献
9.
Itzia I. Padilla-Martínez Noemí Andrade-Lpez Miguel Gama-Goicochea Erndira Aguilar-Cruz Alejandro Cruz Rosalinda Contreras Hugo Tlahuext 《Heteroatom Chemistry》1996,7(5):323-335
1,3,2-Benzimidazaborole, 1,3,2-benzoxaborole, and 1,3,2-benzothiazaborole were synthesized from the corresponding 2-benzazole N(SINGLE BOND)BH3 and 2-benzazole S(SINGLE BOND)BH3 adducts through a reductive transposition from the isolobal fragment X(SINGLE BOND)C(sp2) (DOUBLE BOND) N(sp2) (SINGLE BOND) B(sp3) (X (DOUBLE BOND) N, O, S) to the fragment X(SINGLE BOND)B(sp2) (DOUBLE BOND) N(sp2) (SINGLE BOND) C(sp3). N(SINGLE BOND)BH3 substitution shifts to lower frequencies 4-H, C-3a, and C-7a resonances. The X-ray diffraction analysis of 2-(o-methoxyphenyl)benzothiazole N(SINGLE BOND)BH3 adduct is reported. Two new tetracyclic boron-bridged compounds were observed as by-products (6,9-(ethyl)-diaza-2-oxa-1-bora[3,4,7,8]-dibenzobycyclo[4.3.0]-nona-3,7-diene, 6d, and 8-aza-9-oxa-2-thia-1-bora-[3,4,7,8]dibenzobycyclo[3.4.0]nona-3,7-diene, 15d, when 2-(o-methoxyphenyl)-1-ethylbenzimidazole-BH3 6b and 2-(o-methoxyphenyl)-benzothiazole-BH3 15b adducts were heated. © 1996 John Wiley & Sons, Inc. 相似文献
10.
Bernd Wrackmeyer Christian Khler Wolfgang Milius Jean Michel Grevy Zureima García‐Hernndez Rosalinda Contreras 《Heteroatom Chemistry》2002,13(7):667-676
The preferred conformation of aminophosphanes with bulky amino groups ( 1–20 ) was determined by NMR spectroscopy in solution, in two cases in the solid state ( 11,17 ) and in one case ( 11 ) by X‐ray crystallography. Trimethylsilylaminodiphenylphosphanes Ph2PN(R)SiMe3 (R = Bu ( 1 ), Ph ( 2 ), 2‐pyridyl ( 3 ), 2‐pyrimidyl ( 4 ), Me3Si ( 5 )), amino(chloro)phenylphosphanes Ph(Cl)PNRR′ (R = Bz, R′ = Me ( 6 ), R = Bz, R′ = tBu ( 7 ), R = Et, R′ = Ph ( 8 )), amino(chloro)tert‐butylphosphanes tBu(Cl)PNRR′ (R = R′ = iPr ( 9 ), R = Me, R′ = tBu ( 10 ), R = Bz, R′ = tBu ( 11 ), R = H, R′ = tBu ( 12 ), R = Et, R′ = Ph ( 13 ), R = iPr, R′ = Ph ( 14 ), R = Bu, R′ = Ph ( 15 ), R = Bz, R′ = Ph ( 16 ), R = R′ = Ph ( 17 ), R = R′ = Me3Si ( 18 )), 3‐tert‐butyl‐2‐chloro‐1,3,2‐oxazaphospholane ( 19 ), and benzyl(tert‐butyl)aminodichlorophosphane ( 20 ) were studied by 1H, 13C, 15N, 29Si, and 31P NMR spectroscopy. In all cases, the more bulky substituent at the nitrogen atom prefers the syn‐position with respect to the assumed orientation of the phosphorus lone pair of electrons. Many of the derivatives studied adopt this preferred conformation even at room temperature. Numerous signs of coupling constants 1J(31P, 15N), 2J(31P, 13C), and 2J(31P, 29Si) were determined. Low temperature NMR spectra were measured for derivatives for which rotation about the P N bond at room temperature is fast, showing the presence of two rotamers at low temperature. The respective conformation of these rotamers could be assigned by 13C, 15N, and 31P NMR spectroscopy. Isotope‐induced chemical shifts 1Δ15/14N(31P) were determined for all compounds at natural abundance of 15N by using Hahn‐echo extended polarization transfer experiments. The molecular structure of 11 in the solid state reveals pyramidal surroundings of the nitrogen atom and mutual trans‐positions of the tert‐butyl groups at phosphorus and nitrogen. © 2002 Wiley Periodicals, Inc. Heteroatom Chem 13:667–676, 2002; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.10084 相似文献