155941-72-3Relevant academic research and scientific papers
Synthesis of rhenium(V) 2,4,6-trimethylbenzylidyne complexes by abstracting O2- from an acyl with triflic anhydride
Williams, Darryl S.,Schrock, Richard R.
, p. 2101 - 2104 (2008/10/08)
Re[C(O)Ar′](CO)5 (Ar′ = 2,4,6-C6H2Me3; 1) can be prepared in 55% yield by adding Ar′C(O)Cl to [Re(CO)5]-. Addition of trifluoromethanesulfonic anhydride to 1 in dichloromethane yields off-white [Re-(CAr′)(CO)4(OTf)](OTf) (2) quantitatively. Three equivalents of tetraethylammonium chloride reacts with 2 in dichloromethane to give [Et4N][Re(CAr′)(CO)2Cl3] (3), which when treated with TlBF4 in the presence of pyridine affords lemon yellow Re(CAr′)(CO)2Cl2(py) (4). A slurry of 2 in dichloromethane also reacts cleanly with a THF solution of LiO-2,6-C6H3-i-Pr2 (LiOAr) to yield blood red Re(CAr′)(CO)2(OAr)2(THF) (5a) in 80% isolated yield. Addition of pyridine to 5a yields an analogous six-coordinate pyridine adduct (5b). Addition of pinacol to 2 followed by triethylamine yields yellow, pentanesoluble Re(CAr′)(CO)2(O2C2Me4) (6a). Although 6a shows no tendency to bind THF, it reacts with pyridine to yield Re(CAr′)(CO)2(O2C2Me4)(py) (6b) quantitatively. Addition of triphenylphosphine to 6a produces dark red Re(CAr′)(CO)(O2C2Me4)(PPh3) (6c).
