triethylamine; [Rh(III)(OEP)(Cl)] in tetrahydrofuran a mixt. of NaBH4, Et3N and Rh-catalyst in THF was stirred for 66 h at room temp. under air; ether was added, ppt. filtered, washed with ether, ether ext. and washing were combined, evapd. in vacuo; identified by the IR-spectrum (comparison with authentic sample);
参考文献
Aoyama, Yasuhiro; Fujisawa, Takeshi; Watanabe, Takamichi; Toi, Hiroo; Ogoshi, Hisanobu
Journal of the American Chemical Society, 1986 , vol. 108, # 5 p. 943 - 947
aluminium; aluminium trichloride in neat (no solvent) byproducts: Al(OC6H5)3; High Pressure; heating to 180°C under 2000 psi H2-pressure for 1h; filtration;; separation of product at 97°C and 2 Torr;;
参考文献
Journal of the American Chemical Society, , vol. 84, p. 3407 - 3408
HRh(dmpe)2 in tetrahydrofuran T=50°C; 14 h; Inert atmosphere;
参考文献
Mock, Michael T.; Potter, Robert G.; Camaioni, Donald M.; Li, Jun; Dougherty, William G.; Kassel, W. Scott; Twamley, Brendan; DuBois, Daniel L.
Journal of the American Chemical Society, 2009 , vol. 131, # 40 p. 14454 - 14465
triethyl borane in mineral oil addn. of a small amount of B(C2H5)3 and N(C2H5)3 to NaH in mineral oil at 70°C, addn. of BCl3 at 70-80°C while stirring;; separation by distn.;;
magnesium; mercury dichloride in 2-methyl cyclohexane byproducts: Mg(O-i-C4H9)2; High Pressure; heating to 300°C under 1825 psi H2 pressure;; separation of product by distn.;;
参考文献
Gmelin Handbook: B: B-Verb.14, 3.8.1.2.1, page 94 - 97
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Continental Oil Co.
Patent: US3136820 , 1964 ;
C. A., 1964 , vol. 61, p. 6919
in neat (no solvent) addn. of diborane to amine at liquid N2 temp., keeping at -111°C, -78°C and 0°C consecutively, stirring at 0°C for 4-6 h (vacuum line); cooling to -78°C, removal of B2H6 by distn.;
