scholarly journals Übergangsmetall-Carben-Komplexe, CXXXIV [1]. Synthese neuer Mono- und Biscarben-Komplexe der VI. Nebengruppe; Röntgenstruktur des ersten Bis[amino(alkoxy)carben]-Komplexes / Transition Metal Carbene Complexes, CXXXIV [1]. Synthesis of New Mono- and Bis-Carbene Complexes of Group VIb Elements; Structure of the First Bis[amino(alkoxy)carbene]-Complex

1984 ◽  
Vol 39 (5) ◽  
pp. 668-674 ◽  
Author(s):  
Ernst Otto Fischer ◽  
Rudolf Reitmeier ◽  
Klaus Ackermann

The hexacarbonyl compounds of chromium, molybdenum and tungsten react with the highly nucleophilic agent Li NiPr2 and in a subsequent alkylation with (Et3O)BF4 to give the carbene complexes (CO)5M[C(N′Pr2)OEt] (1, 3, 4). In case of W(CO)6 and Mo(CO)6 the novel biscarbene complexes cis(CO)4M[C(NiPr2)OEt]2 (2, 5) are additionally obtained. Reaction conditions, properties and spectroscopic data of the new compounds are reported. The molecular structure of cis(CO)4W[C(NiPr2)OEt]2 (4) was determined by X-ray crystallography

1983 ◽  
Vol 38 (5) ◽  
pp. 582-586 ◽  
Author(s):  
Ernst Otto Fischer ◽  
Rudolf Reitmeier

AbstractThe cationic carbyne complex [(CO)5WCNEt2]BF4 (1) reacts with potassiumdiphenylamide, KNPh2, with nucleophilic addition of the amide anion to give (CO)5W[C(NEt2)NPh2] (2). The corresponding reactions with KPPh2, KPEt2, KPMePh, NaSbPh2 and NaBiPh2 yield the complex [(CO)5W(CNEt2)]2 (3), which is formed by reductive dimerization of two carbyne fragments. In case of KPMePh the carbene complexes (CO)5W[C(NEt2)PMePh (4) and trans-(MePhPH)(CO)4W[C(NEt2)PMePh] (5) are also obtained. On warming in solution 5 spontaneously rearranges to the novel cyclic carbene complex (6). Reaction conditions, properties and spectroscopic data of the new compounds are reported.


1982 ◽  
Vol 37 (5) ◽  
pp. 627-630 ◽  
Author(s):  
Ernst Otto Fischer ◽  
Paul Rustemeyer

The reaction of Re2(CO)10 with LiSi(C6H5)3 and subsequent alkylation by (C2H5)3OBF4 yields not only (CO)9Re2C(OC2H5)Si(C6H5)3 but also Re1-ax,Re2-eq-[C(OC2H5)Si(C6H5)3]2(CO)8Re2 (1). The analogous isomeric complexes Re1-ax-[C(OC2H5)C6H4CH3]-Re2-eq-[C(OC2H5)Si(C6H5)3](CO)8Re2 (2) and Re1-ax-[C(OC2H5)Si(C6H5)3]-Re2-eq-[C(OC2H5)C6H4CH3](CO)8Re2 (3) are obtained by treatment of eq- or ax-(CO)9Re2C(OC2H5)Si(C6H5)3 with LiC6H4CH3 and subsequent alkylation by (C2H5)3OBF4. Reaction conditions, and properties and spectroscopic data of the new compounds are reported


1980 ◽  
Vol 35 (9) ◽  
pp. 1083-1087 ◽  
Author(s):  
Ernst Otto Fischer ◽  
Paul Rustemeyer ◽  
Dietmar Neugebauer

The reaction between C5H5Re(CO)3 and LiSi(C6H5)3 affords the compound C5H5(CO)2ReC(OCH3)Si(C6H5)3 after subsequent alkylation with CH3SO3F. This complex reacts with BF3 to yield [C5H5(CO)2ReCSi(C6H5)3]BF4. This cationic carbyne complex yields C5H5(CO)2ReC(CH1)Si(C6H5)3 with LiCH3 and C5H5(CO)2ReC(H)Si(C6H5)3 with (C4H9)4NBH4. Reaction conditions, properties and spectroscopic data of the new com­pounds as well as an X-ray structure determination of C5H5(CO)2ReC(H)Si(C6H5)3 are reported.


1982 ◽  
Vol 37 (10) ◽  
pp. 1274-1278 ◽  
Author(s):  
Werner Roll ◽  
Ernst Otto Fischer ◽  
Dietmar Neugebauer ◽  
Ulrich Schubert

The reaction of trans-bromotetracarbonyl(phenylcarbyne)chromium (1) with lithium phenylselenolate and subsequent protonation with aqueous hydrochloric acid leads to (CO)5Cr[Se2(C6H5)2] (3) and (CO)4Cr(μ-SeC6H5)2Cr(CO)4 (4). From 1 and lithium 4-methylphenylthiolate (CO)5CrC(C6H5)SC6H4CH3 (5) and (CO)5CrS(C2H5)(4-CH3C6H4) (6) are obtained, if triethyloxonium tetrafluoroborate is used instead of hydrochloric acid. The analoguous reaction of 1 with lithium phenylselenolate yields the seleno ether complex (7). Reaction conditions, properties, spectroscopic data and the results of an X-ray structure determination of the binuclear complex (4) are reported.


1983 ◽  
Vol 38 (1) ◽  
pp. 67-70 ◽  
Author(s):  
Werner Sieber ◽  
Mathias Wolfgruber ◽  
Dietmar Neugebauer ◽  
Olli Orama ◽  
Fritz R. Kreißl

Abstract Dicarbonyl(η5-cyclopentadienyl)(η1 -cyclopropylketenyl)(trimethylphosphane)tungsten reacts with carbon monoxide under reduction of the ketene moiety forming a (σ-bonded acetylene compound. Reaction conditions, spectroscopic data and the X-ray structure of the new compound are reported.


1985 ◽  
Vol 40 (11) ◽  
pp. 1500-1503 ◽  
Author(s):  
Werner J. Sieber ◽  
Dietmar Neugebauer ◽  
Fritz R. Kreißl

Carbonyl(η5-cyclopentadienyl)(η2-4-methylphenylketenyl)trimethylphosphinetungsten reacts with decaborane(14) under conversion of the η2-ketenyl into a η2-alkyne complex. Reaction conditions, spectroscopic data and the X-ray structure of the new compound are reported.


Molecules ◽  
2019 ◽  
Vol 24 (22) ◽  
pp. 4052 ◽  
Author(s):  
Zainab Almarhoon ◽  
Kholood A. Dahlous ◽  
Rakia Abd Alhameed ◽  
Hazem A. Ghabbour ◽  
Ayman El-Faham

A simple, cost-effective method under environmentally benign conditions is a very important concept for the preparation of 2,3-dihydroquinazolin-4(1H)-one derivatives. The present work describes an efficient and eco-friendly protocol for the synthesis of 2-amino-N-(2-substituted-ethyl)benzamide and 3-substituted-2,3-dihydroquinazolin-4(1H)-one derivatives. The novel feature of this protocol is the use of 2-methyl tetrahydrofuran (2-MeTHF) as an eco-friendly alternative solvent to tetrahydrofuran (THF) in the first step. In the second step, methanol in the presence of potassium carbonate as a catalyst was used under conventional heating or microwave irradiation, which provided an eco-friendly method to afford the target products in excellent yields and purities. NMR (1H and 13C), elemental analysis, and LC-MS confirmed the structures of all compounds. X-ray crystallography further confirmed the structure of the intermediate 2-amino-N-(2-substituted-ethyl)benzamide 3a. The molecular structure of 3a was monoclinic crystal, with P21/c, a = 13.6879 (11) Å, b = 10.2118 (9) Å, c = 9.7884 (9) Å, β = 105.068 (7)°, V = 1321.2 (2) Å3, and Z = 4.


1992 ◽  
Vol 47 (8) ◽  
pp. 1134-1140 ◽  
Author(s):  
Lothar Weber ◽  
Iris Schumann ◽  
Hans-Georg Stammler ◽  
Beate Neumann

The disilylphosphido iron complexes (η5-C5R5)(CO)2Fe-P(SiMe3)2 (1b–d) result from the reaction of the corresponding bromo compounds (η5-C5R5)(CO)2FeBr with LiP(SiMe3)2 · 2 THF. The complexes 2b–d are cleanly converted into the diphosphenyl complexes (η5-C5R5)(CO)2Fe-P=P-Mes* (2b–d) by treatment with equimolar amounts of Mes*PCl2. The products 1b–d and 2b–d have been characterized by elemental analysis as well as spectroscopic data (IR, 1H, 13C, 31P NMR, MS). The molecular structure of η5-C5Me4Et)(CO)2Fe-P(SiMe3)2 (1b) has been established by single-crystal X-ray analysis.


2010 ◽  
Vol 7 (4) ◽  
pp. 1498-1506 ◽  
Author(s):  
S. Goksin Aydinli ◽  
Cemil Ibis

It is known that polyhalogeno-nitro-1,3-butadienes are important starting materials for the synthesis of polyfunctionalized bioactive heterocycles. NovelN,S-substituted nitrobutadienes (4a-j) were synthesized from the reaction of the monothio-substituted nitrodiene derivatives (2a) and (2b) with some piperazine derivatives. These new compounds are stable and the structures of these products were characterized by spectroscopic data. The structure of the novelN,S-substituted nitrodiene compound (4g) synthesized in this study was also elucidated by single crystal x-ray analysis.


1980 ◽  
Vol 35 (6) ◽  
pp. 680-688 ◽  
Author(s):  
Wolfgang A. Herrmann ◽  
Johann Plank ◽  
Ivan Bernal ◽  
Michael Creswick

Abstract The novel doubly bridged μ-methylene iron complexes μ-[C(H)CO2R]-μ-CO[(η5-C5H5)Fe(CO)]2 (R = C2H5: 3a; R = tC4H9: 3b) have been synthesized by low-temperature photolysis of the corresponding alkyldiazoacetates 2a and 2b, resp., in the presence of [(η5-C5H5)Fe(CO)2]2 (1) and characterized by means of their analytical data and IR, 1H NMR and mass spectroscopy. The geometry of 3b has been established by single crystal X-ray diffraction techniques. δ-Alkyl iron complexes of the type (η5-C5H5)Fe(CO)2[CHRRʹ] are accessible from the corresponding diazoalkanes N2 = CRRʹ.


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