1: para-bromotoluene With n-butyllithium in tetrahydrofuran; hexane T=-78 - -10°C; 2: tri-isopropoxy-borane in tetrahydrofuran; hexane T=-78 - 20°C;
参考文献
Lloyd, David G.; Hughes, Rosario B.; Zisterer, Daniela M.; Williams, D. Clive; Fattorusso, Caterina; Catalanotti, Bruno; Campiani, Giuseppe; Meegan, Mary J.
Journal of Medicinal Chemistry, 2004 , vol. 47, # 23 p. 5612 - 5615
magnesium in tetrahydrofuran byproducts: Mg(2+); Electrolysis; electrolysis carried out in a single-compartment cell at room temp., starting materials dissolved in THF containing (CF3SO2)2NLi, solvent and excess B(OiPr)3 evaporated under vacuum, medium hydrolysed at 0°C with an HCl or H2SO4 soln.; extraction with Et2O (3 x 20 ml if the solvent evaporated or 3 x 60 ml otherwise), organic phase dried over sodium or magnesium sulfate and concentrated under vacuum, side product phenol formation avoided by work-up under inert atmosphere;
参考文献
Laza, Carine; Dunach, Elisabet; Serein-Spirau, Francoise; Moreau, Joel J. E.; Vellutini, Luc
New Journal of Chemistry, 2002 , vol. 26, # 4 p. 373 - 375
magnesium in tetrahydrofuran byproducts: Mg(2+); Electrolysis; electrolysis carried out in a single-compartment cell at room temp., starting materials dissolved in THF containing (CF3SO2)2NLi, solvent and excess B(OiPr)3 evaporated under vacuum, medium hydrolysed at 0°C with an HCl or H2SO4 soln.; extraction with Et2O (3 x 20 ml if the solvent evaporated or 3 x 60 ml otherwise), organic phase dried over sodium or magnesium sulfate and concentrated under vacuum, side product phenol formation avoided by work-up under inert atmosphere;
参考文献
Laza, Carine; Dunach, Elisabet; Serein-Spirau, Francoise; Moreau, Joel J. E.; Vellutini, Luc
New Journal of Chemistry, 2002 , vol. 26, # 4 p. 373 - 375
1: With n-butyllithium in tetrahydrofuran; hexane; water T=-78 - 40°C; 2.66667 h; Inert atmosphere; 2: With hydrogenchloride in tetrahydrofuran; hexane; water
