in benzene educt slurried in benzene, B2H6 bubbled through soln. for 24 h; purged with Ar, evapd. in vac., chromd. (SiO2, benzene/heptane), concd.in vac., filtered, dried in vac.;
参考文献
Zheng, Limin; Baker, R. Thomas; Knobler, Carolyn B.; Walker, John A.; Hawthorne, M. Frederick
Inorganic Chemistry, 1983 , vol. 22, p. 3350 - 3355
in dichloromethane-d2 byproducts: H2, P(C6H5)3; dropwise addn. of soln. of catecholborane to soln. of Rh-complex; not isolated; (1)H-, (11)B- and (31)P-NMR spectroscopy; further products;
参考文献
Journal of the American Chemical Society, , vol. 114, # 24 p. 9350 - 9359
in dichloromethane N2-atmosphere; slight stoich. excess of phosphine, refluxing for 14 h; filtration through SiO2, repeated thin layer chromy. (SiO2, Et2O/pentane, then CH2Cl2/pentane); yield depending on details of chromy.; elem. anal.;
in THF-d8 (tetrahydrofuran-d8) byproducts: P(C6H5)3; addn. of soln. of catecholborane to soln. of Rh-complex and oct-1-ene (-78°C, NMR tube), warming (-40°C, (31)P-NMR monitoring), warming to 25°C; (11)B-NMR spectroscopy;
参考文献
Journal of the American Chemical Society, , vol. 114, # 24 p. 9350 - 9359
1: oxalyl dichloride / toluene / 0.5 h / 20 °C / Inert atmosphere 2: sodium tetrahydroborate / diethylene glycol dimethyl ether / 1 h / 20 °C View Scheme
参考文献
Chemical Communications, , vol. 48, # 6 p. 817 - 819
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反应条件
triphenylphosphine in tetrahydrofuran N2-atmosphere; stirring of 2 equiv. of borate, 2 equiv. PPh3 and 1 equiv. of HgCl2 (overnight); filtration, solvent removal (vac.); (11)B-NMR spectroscopy;
