Cui, Yanjie; Abouimrane, Ali; Lu, Jun; Bolin, Trudy; Ren, Yang; Weng, Wei; Sun, Chengjun; Maroni, Victor A.; Heald, Steve M.; Amine, Khalil
Journal of the American Chemical Society, 2013 , vol. 135, # 21 p. 8047 - 8056
trifluoroacetic acid in tetrahydrofuran addn. of known excess of Et3BHLi to N,N-dimethylaminoarenetricarbonylchromium (THF, room temp.), stirring (several h, N2), addn. to a soln. of CF3CO2H (THF, excess); extn., neutralization, sepn. (silica gel flash chromy.), recrystn. (acetone/light petroleum);
in tetrahydrofuran FeCl3 in THF was added dropwise to stirring soln. of 12 ml LiBEt3H in THF (1.0 M), held at const. temp. under N2 atm.; forms of particles dependon dropping rate (1 drop/10s, 1/s, 2/s), stirring rate (200, 400, 1600 rpm) and temp.(0 - 60°C); vac. filtration, washed THF/EtOH (1:1), dried in vac.;
参考文献
Takeuchi, Kenneth J.; Marschilok, Amy C.; Bessel, Carol A.; Dollahon, Norman R.
Journal of Catalysis, 2002 , vol. 208, # 1 p. 150 - 157
carbon monoxide in tetrahydrofuran under N2, THF soln. of Mn complex cooled to -78°C, flushed with CO for 10 min, 1.3 equiv LiBHEt3 added dropwise with stirring under CO, soln. stirred for 10 min at -78°C, slowly warmed to room temp., stirred under CO for 2 h; not isolated, detected by IR;
