192699-83-5Relevant academic research and scientific papers
Preparation and characterization of the rhenium silyl esters (η5-C5Me5)(CO)(NO)ReC(O)OSiR3 (SiR3 = SiMe2Ph, SiEt3)
Cavanaugh, Marisa DiBiase,Tetrick, Stephen M.,Masi, Christopher J.,Cutler, Alan R.
, p. 41 - 48 (1997)
Three synthetic approaches to the rhenium silyl esters Cp * (CO)(NO)ReC(O)OSiEt3 (3) and Cp * (CO)(NO)ReC(O)OSiMe2Ph (4) were evaluated. (a) Treatment of a CH2Cl2 solution of Cp * (CO)2(NO)Re+BF-4 with a silanolate NaOSiEt3 (5) or NaOSiMe2Ph (6) provided 90% isolated yields of 3 and 4. These stable orange-yellow solids are extremely moisture sensitive: traces of water hydrolyze them to Cp * (CO)(NO)ReCO2H and the parent silanol. IR and NMR spectral data of 3 and 4 are consistent with nonchelating μ(η1-C:η1-O) metalloester structures. Less efficient preparative routes to 3 and 4 include treatment of (b) Cp * (CO)(NO)ReCO2H with the requisite chloroalkylsilane and NiPr2Et, and (c) Cp * (CO)(NO)ReCO-2Na+ (7Na+) with the chloroalkylsilane. The new rhenium CO2 adducts Cp * (CO)(NO)ReCO-2M+ (7Li+, 7Na+) were generated by deprotonation of Cp * (CO)(NO)ReCO2H with excess LiH or NaH THF suspensions at 0°C. Both 7Li+ and 7Na+ were characterized by their solution IR spectra and by the formation of their derivatives with silyl and tin chlorides.
