Microwave Accelerated Synthesis of Cyclopentadienyl Bis-Phosphine Ruthenium (II) Thiolato Complexes Using Focused Microwave Irradiation

Abstract

The synthesis of cyclopentadienyl bis-phosphine ruthenium thiolato complexes of the type [RuCp(dppm)SR] from [RuCp(PPh3)2 Cl] using conventional heating and microwave irradiation using a focused monomode reactor is described and the protocols compared. A considerable decrease of the reaction time is observed under microwave conditions. Yields by both methods are comparable. Functionalities such as esters, carboxylic acids and amides on the thiolato ligands are tolerated under the reaction conditions.

Half-sandwich ruthenium complexes of pentafluorobenzenethiolato ligands

“…Cyclopentadienyl ruthenium thiolate complexes containing phosphine ligands are known in the literature [8][9][10][11][12][13][14][15]. They have been made by metathesis reactions of the corresponding chlorides with a variety of thiolate donors [8][9][10][11].…”

“…They have been made by metathesis reactions of the corresponding chlorides with a variety of thiolate donors [8][9][10][11]. The complexes CpRu(PPh 3 ) 2 SR are made by refluxing CpRu(PPh 3 ) 2 Cl and thiolate anions for short times [8,9].…”

“…They have been made by metathesis reactions of the corresponding chlorides with a variety of thiolate donors [8][9][10][11]. The complexes CpRu(PPh 3 ) 2 SR are made by refluxing CpRu(PPh 3 ) 2 Cl and thiolate anions for short times [8,9]. The reactions of these complexes with two-electron donor ligands, L (L = CO, PR 3 , P(OR) 3 ), produced either the mono-(CpRu(PPh 3 )(L)SR) or the di-substituted complexes (CpRu(L) 2 SR) [10][11][12].…”

Indenyl complexes of ruthenium containing thiolate ligands. Structure of IndRu(dppe)SPh

“…The reactivity of compounds containing the CpRu(L) 2 -fragment with sulfur ligands has been extensively studied [19][20][21][22][23][24][25]. The thiolate complexes CpRu(L)(L¢)SR [L, L¢ = PR 3 , P(OR) 3 , CO, dppm, dppe] were made by simple substitution reactions of the corresponding chloride with thiolate anions [19][20][21][22][23][24][25].…”

Microwave-Assisted Synthesis of Coordination and Organometallic Compounds

“…www.intechopen.com using conventional heating and MW using a focused monomode reactor was described (Kuhnert & Danks, 2002). Sealed tube microwave dielectric heating of diaryl acetylenes with cyclopentadienyl Co dicarbonyl at elevated temperature in p-xylene provided access to metallocenes in both the cyclobutadiene (Ar 4 C 4 CoCp, 3-52% yields) and cyclopentadienone (Ar 4 C 4 (CO)CoCp, 14-85% yields) families (Harcourt et al, 2008).…”