Metallkomplexe mit Tetrapyrrol-Liganden, LVI [1] / Metal Complexes with Tetrapyrrole Ligands, LVI [1]

1990 ◽  
Vol 45 (4) ◽  
pp. 531-542 ◽  
Author(s):  
Johann W. Buchler ◽  
Jürgen Löffler
Keyword(s):  
Cyclic Voltammetry ◽  
Metal Complexes ◽  
Mass Spectra ◽  
Electronic System ◽  
Porphyrin Ring ◽  
H Nmr ◽  
Double Decker ◽  
Porphyrin Rings

The reaction of tris(2,4-pentanedionato)europium(III) with a porphyrin H2(P)** in boiling 1,2,4-trichlorobenzene affords a so-called “redox mixture” of europium(III) bisporphyrinates, i. e. porphyrin π-radicals of the type Eu(P)2 and sandwiches EuH(P)2 in which one of the porphyrin rings is protonated. Thus, from either tetraphenylporphyrin or its dilithium derivative, or octaethylporphyrin, or a mixture of both porphyrins, the corresponding mixtures of double-deckers with two identical or two differnt porphyrin rings are obtained. The transformation of the redox mixtures into the pure tetraphenylporphyrin derivatives Eu(TPP)2, EuH(TPP)2, and the salt [NBu4] [Eu(TPP),, the separation of the octaethylporphyrin derivatives Eu(OEP)2 and EuH(OEP)2, and the purification of the “mixed” double-decker Eu(OEP)-(TPP) are described. The compounds are characterized by cyclic voltammetry, IR, UV/VIS/NIR, 1H NMR, and mass spectra. The obtained data indicate that the π-electrons of the two porphyrin rings behave as a common electronic system in which a defect electron is delocalized. However, in the “mixed” double-decker Eu(OEP) (TPP) the defect electron is more concentrated on the OEP ring, i. e. the porphyrin ring which is more easily oxidized.

Metallkomplexe mit Tetrapyrrol-Liganden, XXVIII. Mononukleare Nitridomangan(V)-Porphyrine: die ersten Mangan-Stickstoff-Dreifachbindungen/ Metal Complexes with Tetrapyrrole Ligands, XXVIII. Mononuclear Nitridomanganese(V) Porphyrins: the First Manganese Nitrogen Triple Bonds

1982 ◽  
Vol 37 (9) ◽  
pp. 1155-1162 ◽  
Author(s):  
Johann W. Buchler ◽  
Christine Dreher ◽  
Kiong Lam Lay
Keyword(s):  
Metal Complexes ◽  
Triple Bond ◽  
Mass Spectra ◽  
H Nmr ◽  
Triple Bonds

AbstractThe first complexes containing a manganese-nitrogen triple bond, nitrido(octaethylporphinato) manganese(V) [MnN(OEP)]** and nitrido[meso-tetra(p-tolyl)porphinato]manganese( V) [MnN(TTP)], are prepared by hypochlorite oxidation of the corresponding methoxomanganese( III) porphyrins, Mn(OEP)OMe and Mn(TTP)OMe, in the presence of ammonia. The red, pentacoordinated, diamagnetic species are identified by UV/VIS-, IR-, 1H NMR, and mass spectra. While the isoelectronic oxochromium(IV) or oxomolybdenum( IV) porphyrins behave as weak oxidants or reductants, respectively, the nitridomanganese( V) unit in the square pyramidal environment is chemically remarkably stable.

Metallkomplexe mit Tetrapyrrol-Liganden, XXXI [1]. Neutrale und anionoide Bisporphinate des Gers und Praseodyms / Metal Complexes with Tetrapyrrole Ligands, XXXI [1]. Neutral and Anionoid Bisporphinates of Cerium and Praeseodymium

1983 ◽  
Vol 38 (11) ◽  
pp. 1339-1345 ◽  
Author(s):  
Johann W. Buchler ◽  
Heinz-Günter Kapellmann ◽  
Martina Knoff ◽  
Kiong-Lam Lay ◽  
Stefan Pfeifer
Keyword(s):  
Metal Complexes ◽  
Mass Spectra ◽  
Conductivity Measurements ◽  
H Nmr ◽  
Sandwich Type

Abstract The preparation of the lanthanoid bisporphinates, bis[meso-tetra(p-tolyl)porphinato]-cerium(IV) [Ce(TTP)2**] and bis[meso-tetra(p-tolyl)porphinato]hydrogenpraseodymium-(III) [PrH(TTP)2] from Ce(acac)3 and Pr(acac)3 in boiling 1,2,4-trichlorobenzene is described. Ce(TTP)2 is a diamagnetic and rather inert CeIV derivative, PrH(TTP)2 is a paramagnetic PrIII complex and may be deprotonated to give the anion [Pr(TTP)2]- which is characterized by conductivity measurements, electrophoresis, and isolation of its tetra(n-butyl)ammonium or tetraphenylarsonium salt. The compounds are identified by UV/VIS, IR, 1H NMR, and mass spectra. The data are consistent with a sandwich-type square antiprismatic array of the two porphinate disks about the CeIV or PrIII ion as found earlier in the bis-phthalocyaninates U(Pc)2 or NdH(Pc)2.

scholarly journals Synthesis, Characterization and Antibacterial Activity of Novel Schiff Bases Derived from 4-Phenyl-2-aminothiazole and their Mn(II), Fe(II), Co(II), Ni(II) and Cu(II) Metal complexes

2011 ◽  
Vol 8 (4) ◽  
pp. 1556-1565 ◽  
Author(s):  
A. S. Thakar ◽  
K. S. Pandya ◽  
K. T. Joshi ◽  
A. M. Pancholi
Keyword(s):  
Antibacterial Activity ◽  
Metal Complexes ◽  
Schiff Bases ◽  
Mass Spectra ◽  
Uv Spectra ◽  
Assay Method ◽  
H Nmr ◽  
Ft Ir ◽  
Schiff Base Metal Complexes ◽  
C Nmr

Novel Schiff bases and their metal complexes were derived from some hetero cyclicβ-diketones with 4-phenyl-2-aminothiazole. All the synthesized compounds were confirmed their structure by Elemental analysis, FT-IR,1H NMR,13C NMR, Mass spectra, TGA analysis and UV spectra. All the compounds were tested for their antibacterial activity. Spectroscopic measurements suggest that all Schiff base metal complexes are of type ML2.(H2O)2(M=Mn, Fe, Co, Ni and Cu) and all the metal complexes shows moderate antibacterial activity in the agar cup assay method.

Metal Complexes with Tetrapyrrole Ligands, LV [ 1 ] Improved Syntheses of Oxorhenium(V) Porphyrins and Novel Trichlororhenium(V) Porphyrins

1990 ◽  
Vol 45 (4) ◽  
pp. 518-530 ◽  
Author(s):  
Johann W. Buchler ◽  
Steffen B. Kruppa
Keyword(s):  
Acetic Acid ◽  
Organic Acids ◽  
Metal Complexes ◽  
Alkaline Hydrolysis ◽  
Mass Spectra ◽  
Efficient Synthesis ◽  
H Nmr ◽  
Primary Products ◽  
Metal Insertion ◽  
Alkali Salts

The reaction of ReCl5 with a porphyrin H2(P) [2, 3] in refluxing trichlorobenzene represents a very efficient synthesis of oxorhenium(V) porphyrins ReO(P)X where X is a uninegative anion. Thus, rhenium is inserted to octaethylporphyrin and a variety of tetraarylporphyrins. The primary products are the paramagnetic trichlororhenium(V) porphyrins, ReCl3(P), which are remarkably resistant to hydrolysis. If moisture is not rigorously excluded from the metal insertion system, chlorooxorhenium(V) porphyrins ReO(P)Cl are formed which during alumina chromatography are converted to the methoxides ReO(P)OMe. All complexes ReO(P)X and ReCl3(P) are subject to alkaline hydrolysis yielding the μ-oxo complexes [ReO(P)]2O which are convenient starting materials for a variety of mononuclear species ReO(P)X [X = OMe, OEt, OiPr, OtBu, F, Cl, Br, OCIO3, OAc, OBz, OCN, NCS] on acidolysis with a number of monobasic inorganic and organic acids HX or reaction with alkali salts MX in presence of acetic acid. In the case of tetramesitylporphyrin, hydrolysis yields a mononuclear hydroxooxorhenium(V) porphyrin. The species ReCl3(P) and ReO(P)X are characterized by UV/VIS, IR, 1H NMR and mass spectra.

Templated tetramerization of dicyanobenzenes to form mixed porphyrinato and phthalocyaninato rare earth(III) triple-decker complexes

2002 ◽  
Vol 06 (05) ◽  
pp. 347-357 ◽  
Author(s):  
Na Pan ◽  
Jianzhuang Jiang ◽  
Xuegui Cui ◽  
Dennis P. Arnold
Keyword(s):  
Rare Earth ◽  
Comparative Study ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
Aromatic Proton ◽  
Organic Base ◽  
H Nmr ◽  
Near Ir ◽  
Double Decker

Heteroleptic porphyrinato/phthalocyaninato rare earth(III) triple-decker compounds M 2( Por )2( Pc ') (1a-4a) and M 2( Por )( Pc ')2 (1c-4c) ( M = Eu , Tb ; Por = TDOPP , Pc ' = OOPc or Por = TpClPP , Pc ' = Pc where H 2(TDOPP) = 5,10,15,20-tetrakis(4-n-dodecyloxyphenyl)porphyrin, H2[OOPc] = 2,3,9,10,16,17,23,24-octakis(n-octyloxy)phthalocyanine, H 2(TpClPP) = 5,10,15,20-tetrakis(4-chlorophenyl)porphyrin, H 2( Pc ') = general phthalocyanine, and H 2( Pc ) = unsubstituted phthalocyanine) were obtained by the cyclic tetramerization of the corresponding dicyanobenzenes 7 using monoporphyrinato rare earth(III) acetylacetonates M(Por)acac as templates with catalysis by the organic base 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU). Double-decker complexes M(Por)(Pc') ( M = Eu , Tb ; Por = TDOPP , Pc ' = OOPc or Por = TpClPP , Pc ' = Pc ) (1b-4b) were isolated as side products. For the purpose of comparative study, homo- and hetero-dinuclear rare earth triple-deckers with one porphyrinato and two phthalocyaninato ligands M2(Por)( Pc ')2 (1c, 2c) ( M = Eu , Tb ; Por = TDOPP , Pc ' = OOPc ) and ( Por ) M ( Pc ') M '( Pc ')( M ≠ M ' = Eu , Tb ) (5c, 6c) were also prepared using the raise-by-one-story method. The complexes were characterized by UV-vis, near-IR, IR and mass spectra. The comparison between 1 H NMR spectra of the two series of triple-decker compounds a and c, and also between the substituted phthalocyanine- and unsubstituted phthalocyanine-containing europium triple-deckers, renders it possible to assign the aromatic proton signals unambiguously.

Synthesis of 2-amino-5,7-dimethyl-4-oxopyrido[3,4-e]-1,3-thiazines

1983 ◽  
Vol 48 (12) ◽  
pp. 3426-3432 ◽  
Author(s):  
Dušan Koščík ◽  
Pavol Kristian ◽  
Ondrej Forgáč
Keyword(s):  
Spectral Data ◽  
Chlorine Atom ◽  
Mass Spectra ◽  
High Reactivity ◽  
Secondary Amines ◽  
Dimroth Rearrangement ◽  
H Nmr ◽  
New Synthesis ◽  
C Nmr

New synthesis of pyrido[3,4-e]-1,3-thiazines consisting in reaction of 2,6-dimethyl-4-chloronicotinoyl isothiocyanate with primary or secondary amines, or with benzaldehyde phenylhydrazone, is described. High reactivity of the chlorine atom does not allow isolation of the corresponding thioureas, arising as intermediates, except in the case of the benzylamino derivative. Structure of the products was unequivocally confirmed by their spectral data (IR, UV, 1H NMR, 13C NMR and mass spectra). The synthesized derivatives do not undergo the Dimroth rearrangement.

Preparation, properties and structure of some intermediate nido- and arachno-monocarbaboranes

1981 ◽  
Vol 46 (10) ◽  
pp. 2345-2353 ◽  
Author(s):  
Karel Baše ◽  
Bohumil Štíbr ◽  
Jiří Dolanský ◽  
Josef Duben
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Nmr Spectra ◽  
Liquid Ammonia ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Starting Compound

The 6-N(CH3)3-6-CB9H11 carbaborane reacts with sodium in liquid ammonia with the formation of 6-CB9H12- which was used as a starting compound for preparing the 4-CB8H14, 9-L-6-CB9H13 (L = (CH3)2S, CH3CN and P(C6H5)3), 1-(η5-C5H5)-1,2-FeCB9H10-, and 2,3-(η5-C5H5)2-2,31-Co2CB9H10- carboranes. The 4-CB8H14 compound was dehydrogenated at 623 K to give 4-(7)-CB8H12 carborane. Base degradation of 6-N(CH3)3-6-CB9H11 in methanol resulted in the formation of 3,4-μ-N(CH3)3CH-B5H10. The structure of all compounds was proposed on the basis of their 11B and 1H NMR spectra and X-ray diffraction was used in the case of the transition metal complexes.

Oxynemorensine, an alkaloid from Senecio nemorensis L., var. subdecurrens GRISEB

1980 ◽  
Vol 45 (2) ◽  
pp. 548-558 ◽  
Author(s):  
Antonín Klásek ◽  
Petr Sedmera ◽  
Jindřich Vokoun ◽  
Anna Boeva ◽  
Svatava Dvoráčková ◽  
...  
Keyword(s):  
Unsaturated Acid ◽  
Mass Spectra ◽  
H Nmr ◽  
C Nmr

From S. nemorensis L., var. subdecurrens GRISEB. there were isolated the previously obtained alkaloids nemorensine (I), retroisosenine (II), bulgarsenine (III) and, in addition, the alkaloid oxynemorensine which was assigned the structure VIII on the basis of the interpretation of the 1H-NMR, 13C-NMR, mass spectra, and on that of the identification of the products of hydrolysis and reduction. Furthermore, the isolation of the cis-nemorensic acid (V) as well as that of the unsaturated acid IV, and the transformation of bulgarsenine (III) to nemorensine (I) were described.

Synthesis and Antibacterial Properties of Some 4-Amino Substituted 2-Phenyl-6H-5,1,3-benzothiadiazocines

1996 ◽  
Vol 61 (11) ◽  
pp. 1681-1688 ◽  
Author(s):  
Michal Bodajla ◽  
Štefan Stankovský ◽  
Katarína Špirková ◽  
Soňa Jantová
Keyword(s):  
Mass Spectra ◽  
Antibacterial Properties ◽  
H Nmr ◽  
Antibacterial Screening

Some 4-amino substituted 2-phenyl-6H-5,1,3-benzothiadiazocines (4a-4j) were prepared by cyclization of the corresponding N1-[N-(2-chloromethylphenyl)benzimidoyl]-N2-substituted thioureas (3a-3j). The IR,1H NMR and mass spectra of the title compounds are reported together with the results of antibacterial screening.

scholarly journals Isocyanate und verwandte Verbindungen des trimeren Phosphornitriddifluorids / Isocyanates and Related Compounds of Trimeric Phosphor-difluoronitride

1971 ◽  
Vol 26 (7) ◽  
pp. 679-683 ◽  
Author(s):  
Herbert W. Roesky ◽  
Enno Janssen
Keyword(s):  
Ir Spectra ◽  
Elemental Analysis ◽  
Mass Spectra ◽  
H Nmr ◽  
Carbonic Acids ◽  
Related Compounds

P3N3F5NCO was prepared by reaction of P3N3F5NSO with (COCl) 2. Substituted amides were obtained from the reaction of P3N3F5NSO with carbonic acids e. g. P3N3F5NHCOCH3, P3N3F5NHCOC2H5, and P3N3F5NHCOC3H7. If these substances were treated with PCl5 the following compounds P3N3F5N = CClCH3, P3N3F5N = CClCH5, and P3N3F5TN = CClC3H7 were formed. They reacted with nucleophiles to give P3N3F5N = CNH2CH3, P3N3F5N = TN (CH3) 2C2H5, and P3N3F5N = CN (CH3) 2CH7. The properties of these compounds are described. They were characterized by elemental analysis and IR-spectra. 19F-, 1H-NMR, and mass spectra are reported.

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