A convenient route for the preparation of the monohydride catalyst trans-[RuCl(H)(dppe)2] (dppe=Ph2PCH2CH2PPh2): Improved synthesis and crystal structure

• Published in: Inorganic chemistry communications 2013-03, Vol.29, p.123-127
• Main Authors: Figueira, João, Jardim, Manuel G., Rodrigues, João, Valkonen, Arto, Rissanen, Kari
• Format: Article
• Language: English
• Subjects: Homogeneous catalysis; Hydrides; Hydrogenation; Ruthenium; Synthetic methods; X-ray crystal structure
• ISSN: 1387-7003; 1879-0259
• DOI: 10.1016/j.inoche.2013.01.002

A novel and improved room temperature synthesis of the monohydride catalyst trans-[RuCl(H)(dppe)2] complex (1, dppe (1,2-bis(diphenylphosphino)ethane)=Ph2PCH2CH2PPh2) proceeds through oxidation of methanol (the solvent) by the pentacoordinated cis-[RuCl(dppe)2][PF6] complex and t-BuOK as the base is described. Compound 1 was fully characterized by NMR (1H, 13C, 31P), ESI-MS(TOF+), FTIR and elemental analysis. The X-ray structure of 1 was reported for the first time and unambiguously confirms the trans-configuration of the complex. A new and easy way to synthesize the trans-[RuCl(H)(dppe)2], (1) in high-yield was presented and its X-ray structure was reported for the first time. [Display omitted] ► A faster way to access the catalyst trans-[RuCl(H)(dppe)2](1) is presented. ► Compound 1 X-ray structure is presented for the first time. ► The synthesis of 1 is a cost effective pathway for the preparation of derivatives. ► Room temp. synthesis of 1 is important in domains beyond catalysis and materials.