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), dried over sodium or magnesium sulfate and concentrated undervacuum, side product phenol formation avoided by work-up under inert at mosphere, recrystallized in CH2Cl2;
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
Qian, Yimin; Marugan, Juan Jose; Fossum, Renae D.; Vogt, Andreas; Sebti, Said M.; Hamilton, Andrew D.
Bioorganic and Medicinal Chemistry, 1999 , vol. 7, # 12 p. 3011 - 3024
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), dried over sodium or magnesium sulfate and concentrated undervacuum, side product phenol formation avoided by work-up under inert at mosphere, recrystallized in CH2Cl2;
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
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), dried over sodium or magnesium sulfate and concentrated undervacuum, side product phenol formation avoided by work-up under inert at mosphere, recrystallized in CH2Cl2;
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
n-butyllithium in tetrahydrofuran N2; BuLi dropping into org. compd. soln. at -78°C, mixt. keeping 3 h, B-compd. soln. addn. dropwise at -78°C, mixt. allowing to warm to room temp. overnight , stirring 1 h with 10percent HCl, extn. (Et2O); org. extracts washing (water), drying, solvent vac. removal;
参考文献
Imrie, Christopher; Loubser, Christa; Engelbrecht, Pieter; McCleland, Cedric W.
Journal of the Chemical Society - Perkin Transactions 1, 1999 , # 17 p. 2513 - 2523
Qian, Yimin; Marugan, Juan Jose; Fossum, Renae D.; Vogt, Andreas; Sebti, Said M.; Hamilton, Andrew D.
Bioorganic and Medicinal Chemistry, 1999 , vol. 7, # 12 p. 3011 - 3024
