hydrogenchloride in xylene below 30°C; reaction mixture pured into ice, organic layer separated, washed with water, aqueous layers are neutralized with 6N HCl;
in neat (no solvent, gas phase) Irradiation (UV/VIS); BCl3/D2 gas mixt. irradiated with CO2 laser beam (up to 1.27 J/cm**2/pulse) at 1-10 Torr pressure; monitored by IR;
参考文献
Lee, Kuk-Haeng; Takeo, Harutoshi; Kondo, Shigeo; Matsumura, Chi
Bulletin of the Chemical Society of Japan, 1985 , vol. 58, # 6 p. 1772 - 1777
Gerrard, W.; Mooney, E. F.; Rees, R. G.
Journal of the Chemical Society, 1964 , p. 740 - 745
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Gmelin Handbook: Sn: Org.Verb.1, 1.1.1.5.4.4, page 104 - 106
in hexane; toluene under N2; soln. of BCl3 (1.00 equiv) in hexanes added to soln. of (Cu(C6F5))4(η2-toluene)2 in toluene at -78 °C; mixt. stirred at -78°C for 1 h and then allowed to gradually warm to room temp.; products not sepd.; product distribution in supernatant estimated by (19)F-NMR spectroscopy;
参考文献
Journal of Organometallic Chemistry, , vol. 681, # 1-2 p. 134 - 142
in dichloromethane under N2; soln. of C6F5Cu in CH2Cl2 added dropwise over 20 min to soln. of BCl3 (3 equiv) in CH2Cl2 at -78 °C; mixt. stirred at -78 °C for 1 h and then allowed to slowly warm to room temp. and stirred for 3 h; after filtration all volatiles slowly removed under high vac. first at -25 °C and subsequently over 3 h at 0 °C; crude product distd. under dynamic vac. at ca. 40 °C into cold trap (liq. N2); vac. transfer into storage flask;
参考文献
Sundararaman, Anand; Jaekle, Frieder
Journal of Organometallic Chemistry, 2003 , vol. 681, # 1-2 p. 134 - 142
