in pyridine byproducts: NaCl; react. in pyridine (exclusion of H2O); filtration, removal of excess C5H5N in vac. at 50°C, pptn. of excess (C5H5NH)Cl by addn. of ether;; 99.8percent purity; (purification also by shaking with H2O);;
参考文献
Journal of the American Chemical Society, , vol. 77, p. 1506
pyridine; [Rh(III)(OEP)(Cl)] in tetrahydrofuran a mixt. of NaBH4, Py and Rh-catalyst in THF was stirred at room temp. under air; ether was added, ppt. filtered, washed with ether, ether ext. and washing were combined, evapd. in vacuo;
参考文献
Journal of the American Chemical Society, , vol. 108, # 5 p. 943 - 947
pyridine in pyridine to NaBH4 in a flask at 10°C is added pyridine, then is slowly added sulfur (2 h); the amine is evapd., to the residue is added benzene, the solvent is after 1 d removed, elem. anal.;
参考文献
Zeitschrift fuer Naturforschung, Teil B: Anorganische Chemie, Organische Chemie, , vol. 38, # 2 p. 203 - 207
pyridine 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.;
in benzene under N2 atm. pyridine was added to soln. ((EtH2N)B8H11NHEt) in benzene and soln. was heated at reflux for 3 h; volatile components were removed in vacuo, residue was redissolved in CH2Cl2 and chromed.;
参考文献
Journal of Organometallic Chemistry, , vol. 614-615, p. 215 - 222
