Structure and reactivity of the arenecarbonyl cation iodotricarbonylhexamethylbenzenetungsten(II)

1969 ◽  
Vol 22 (4) ◽  
pp. 709 ◽  
Author(s):  
MR Snow ◽  
P Pauling ◽  
MHB Stiddard

Substituted carbonyls of the type (arene)M(CO)3 (M = Mo, W) react with iodine to yield compounds containing the cation [(arene)M(CO)3I]+. X-ray structure analysis shows the [(hexamethylbenzene)W(CO)3I]+ species to possess approximate Cs symmetry. It is unstable in solution and reaction with bipyridyl and triphenyl-phosphine offers a new route to derivatives of the type W(bipyridyl)2(CO)3I2 and W(PPh3)2(CO)3I2.

1990 ◽  
Vol 45 (7) ◽  
pp. 985-988 ◽  
Author(s):  
Gabriele Knörzer ◽  
Hermann Seyffer ◽  
Hans Pritzkow ◽  
Walter Siebert

Allyldiboran(4) derivatives la—c are obtained from allylmagnesium chloride and chloro derivatives of diboran(4). la—c are air-sensitive liquids; heating of le did not yield a 2,3-dihydro-l,2-diborole derivative (B). Reaction between 1,1-bis(dichloroboryl)-3,3-dimethyl-butane (5) and H2C=C(CH2SnMe3)2 (4) leads to the heat-sensitive chloro derivative 2a, in which the chlorine is substituted by Me3SiNMe2 to give stable 1,3-bis-dimethylamino-5-methylene-2-neopentyl- 1,3-diborinane (2 b). 1,2-Bis(dichloroboryl)benzene and 4 yield the chloro derivative 3a, and its substitution with HN(i-Pr)2 leads to 1,4-bis(diisopropylamino)-2,3-benzo-6-methylene-1,4,5,7-tetrahydro-1,4-diborepine (3 b). The X-ray structure analysis reveals a folded tetrahydro-1,4-diborepine ring.


1983 ◽  
Vol 61 (2) ◽  
pp. 282-283 ◽  
Author(s):  
Stanley C. Nyburg ◽  
Pik Y. Siew ◽  
Gavin N. Saunders ◽  
John R. Purdy ◽  
Stewart McLean

The structure and absolute configuration of a bisepoxide (2) produced by oxidation of tetraacetylsecologanin dimethyl acetal (1) with m-chloroperbenzoic acid have been established by X-ray crystal structure analysis. Epoxidation of the vinyl side chain is unexceptional; epoxidation of the β-alkoxyacrylate moiety is novel. This determination represents a valuable bench mark for configurational assignments, since the bisepoxide has been correlated by chemical transformations with a number of synthetic and naturally-occurring derivatives of secologanin.


2007 ◽  
Vol 72 (12) ◽  
pp. 1740-1754 ◽  
Author(s):  
Eugen Justus ◽  
Dana T. Izteleuova ◽  
Alexander V. Kasantsev ◽  
Mendel M. Axartov ◽  
Enno Lork ◽  
...  

A series of derivatives of coumarin (2H-chromen-2-one) and 6,7-benzocoumarin (3H-benzo-[f]chromen-3-one) carrying the o-carborane, m-carborane, and dodecaborate clusters, has been obtained. X-ray structure analysis has been carried out for three of the products. The addition of o-carborane occurs in the 4-position of the coumarin ring, in a stereoselective way, independent of whether the cluster was reacted as the lithium or magnesium salt. m-Carborane gives two products, one being the result of 1,2-addition to an exocyclic ester bond and 1,4-addition to the coumarin system, the other resulting from 1,4-addition. The negatively charged dodecaborate derivatives obtained, link the cluster via oxygen or sulfur and an appropriate linker to a 7-hydroxy-substituted coumarin. For the coumarin derivatives, an o-carboranecarbonyl derivative could also be obtained.


Synthesis ◽  
2020 ◽  
Vol 52 (23) ◽  
pp. 3622-3631
Author(s):  
Victor V. Fedotov ◽  
Evgeny N. Ulomsky ◽  
Konstantin V. Savateev ◽  
Evgeny M. Mukhin ◽  
Denis A. Gazizov ◽  
...  

A highly efficient PASE approach to a new class of polycyclic purine derivatives has been proposed. The strategy includes a consecutive reduction, auto-aromatization, and heterocyclization of the initial nitrobenzimidazopyrimidines obtained by a three-component condensation. It was shown that reduction of nitrobenzimidazopyrimidines by metals in acidic media was more efficient than heterogeneous hydro­genation. Novel derivatives of benz[4,5]imidazo[1,2-a]purines were obtained­ in good yields and the proposed structure was confirmed by X-ray crystal structure analysis. The obtained convergent benzimidazopurines combine two relevant medicinal chemistry scaffolds – benz­imidazole and purine.


2008 ◽  
Vol 63 (12) ◽  
pp. 1395-1401 ◽  
Author(s):  
Ulrich Siemeling ◽  
Clemens Bruhn ◽  
Mario Meier ◽  
Christian Schirrmacher

A broad range of azobenzene derivates of the general type I-p-C6H4-N=N-p-C6H4-X (1) have been prepared. In the case of X = Ph (b), C≡C-Fc (e, Fc = ferrocenyl), OMe (g), Oi-Pr (i), and NMe2 (m), these compounds have been characterised by single-crystal X-ray structure analysis. In addition, the closely related 4-dimethylamino-1-(4-iodophenylazo)naphthalene 2 and 8-(4-iodophenylazo) quinoline 3 have also been prepared. Furthermore, the ferrocene derivative Fc-C≡C-p-C6H4- NH2 (4), which served as a starting material for the synthesis of I-p-C6H4-N=N-p-C6H4-p-C6H4- C≡C-Fc (1e), was prepared and structurally characterised by X-ray diffraction.


1980 ◽  
Vol 35 (9) ◽  
pp. 1075-1082 ◽  
Author(s):  
D. Fenske ◽  
H. Prokscha ◽  
P. Stock ◽  
H. J. Becher

With R2PSi(CH3)3 (R = C6H5, i-C3H7, t-C4H9) one Cl atom of 3,4-dichlor-5-methoxy-2(5 H)-furanon (1) is substituted by the R2P group. An x-ray crystal structure analysis of the phosphino derivative with R = C6H5 (2) it has shown that of the two Cl atoms in 1 only the β-position (to C= O) is substituted. The coordination chemistry of 2 and its bis- (diphenylphosphino) derivative (3) is studied by preparation of the compounds 2 · Mo(CO)5 and 3 · Mo(CO)4. With PdCl2 · 2 C6H5CN (2) gives a dinuclear complex [2 · PdCl2]2, with bridging Cl atoms. The structure is established by a comparison with the similar complex of PdCl2 and 2-chloro-diphenylphosphino-maleic acid dimethylestor, which was synthe­sized as a model compound and studied by x-ray crystal structure analysis.


2013 ◽  
Vol 11 (12) ◽  
pp. 2144-2150 ◽  
Author(s):  
Anastasiia Mishura ◽  
Anna Sklyarova ◽  
Dmitriy Sharapa ◽  
Igor’ Levandovsky ◽  
Michael Serafin ◽  
...  

AbstractThe rearrangement of easily accessible Cookson’s diketone with chlorosulfonic acid in chloroform followed by the acidic hydrolysis gave 6-chloro-7-hydroxy-dichloropentacyclo[6.3.0.02,6.03,10.05,9]undecane-4-one, whose syn-stereochemistry was assigned through the X-ray crystal structure analysis. This key structure was used for the stereoselective synthesis of the D 3-trishomocubane derivatives as well as for the preparation of potential drugs bearing hydroxy- and amino-functional groups. A new multigram preparative synthesis of D 3-trishomocubane was developed.


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