Synthesis of cyclopentadienyltricarbonylrhenium(I) carboxylic acid from perrhenate

Amino acid-functionalized cyclopentadienyl molybdenum tricarbonyl complex and its use in catalytic olefin epoxidation

“…Solvents were dried by standard procedures (n-hexane, diethyl ether and THF with Na/benzophenone ketyl; dichloromethane with CaH 2 ), distilled under nitrogen and used immediately (for THF) or kept over 4 Å molecular sieves. Cyclopentadienyllithium (CpLi) was synthesized as described previously [17]. N-benzyloxycarbonyl-l-proline was purchased from Panreac and hydroxybenzotriazole (HOBT), dicyclohexylcarbodiimide (DCC), urea hydrogen peroxide (UHP) and 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]BF 4 ) from Fluka.…”

Synthesis and properties of carboxy-substituted half-sandwich ruthenium complexes with chelating bisphosphine ligands (η5-C5H4CO2H)Ru(η2-L)X (X=I, H)

“…Three routes to C 5 H 4 CO 2 H complexes have been reported: (a) Cp ligands can be lithiated and treated with CO 2 [3], (b) C 5 H 4 CO 2 Me complexes can be prepared and the ester saponified [4], and (c) C 5 H 4 CO 2 H complexes can be prepared directly from the free ligand (Thiele's acid) [5,6]. However, we have found that none of these methods work for the preparation of (g 5 -C 5 H 4 CO 2 H)Ru(g 2 -L)X (Table 1), so we have tried a variant of (b) that avoids strong base: the preparation of complexes of the corresponding t-butyl esters and the use of trimethylsilyl iodide to effect their hydrolysis [7].…”

The [Re(CO)6]+ Cation as a Ligand-Transfer Reagent with Ferrocene Derivatives

“…The search for an efficient preparation method has led us to propose a new synthesis for certain rhenium compounds, including Re 2 (CO) 10 at normal atmospheric pressure, [12] and (η 5 -C 5 H 4 COOH)Re(CO) 3 by a simple thermal reaction of Re 2 (CO) 10 . [13] Other synthetic advances have been made by Katzenellenbogen et al [14] and by Alberto et al [15] Recently, Alberto demonstrated the viability of preparing cyclopentadienyltechnetium complexes in aqueous media using the reagent [Tc(CO) 3 (H 2 O) 3 ] ϩ obtained from radioactive pertechnetate. [16] However, this synthesis is limited for the moment to cyclopentadienyl compounds bearing a carbonyl substituent.…”

“…ϪNHϪCO) ppm 13. C NMR (100 MHz, (CD 3 ) 2 CO): δ ϭ 86.6 (C Cp ), 88.1 (C Cp ), 96.5 (C Cp ), 120.9 (C Ar ), 124.7 (C Ar ), 129.4 (C Ar ), 139.3 (C Ar ), 161.0 (NHCϭO), 194.1 (CO) ppm.…”