hydrogenchloride; water in tetrahydrofuran (Ar); stirring (-30°C), stirring (room temp., overnight), hydrolysis (0°C, water, 4M HCl), evapn. of the solvent, extn. (ether); evapn. of the solvent, recrystn. (water); elem. anal.;
参考文献
Norrild, Jens Chr.; Eggert, Hanne
Journal of the American Chemical Society, 1995 , vol. 117, # 5 p. 1479 - 1484
aluminium in N,N-dimethyl-formamide byproducts: Al(3+); Electrolysis; electrolysis carried out in a single-compartment cell at room temp., starting materials dissolved in DMF containing KBr or n-Bu4NBr, solvent andexcess B(OCH3)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
magnesium in N,N-dimethyl-formamide byproducts: Mg(2+); Electrolysis; electrolysis carried out in a single-compartment cell at room temp., starting materials dissolved in DMF containing KBr or n-Bu4NBr, solvent andexcess B(OCH3)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: 2-bromo-1-methoxy-4-methyl-benzene With n-butyllithium in tetrahydrofuran T=-78°C; 1 h; 2: boric acid trimethyl ester in tetrahydrofuran T=-78 - 20°C; 4 h; 3: With hydrogenchloride in tetrahydrofuran; water
参考文献
Erickson-Miller, Connie J; Eppley, Daniel F.; Jenkins, Julian; Luengo, Juan I.; Liu, Nannan; Price, Alan T.; Shaw, Anthony N.; Visonneau, Sophie; Wiggall, Kenneth
Patent: US2004/19190 A1, 2004 ;
Location in patent: Page 24 ;
