magnesium in tetrahydrofuran byproducts: MgBrCl; (Ar), Sb-compd. in THF added to Mg-chips, Me3SiCl added dropwise, stirred for 1 h; THF removed at 0.1 mmHg, washed several times with pentane, removed, distilled at 155°C/0.01 mmHg;
参考文献
Zeitschrift fuer Naturforschung, Teil B: Anorganische Chemie, Organische Chemie, , vol. 37, # 4 p. 395 - 400
pyridine; cyclohexanone in tetrahydrofuran; toluene byproducts: methylenecyclohexane; mixt. of soln. of Ti complex (1 equiv.) in THF/toluene and cyclohexanonewas heated at 80-85°C for 6 h under Ar; cooled to room temp.; py ridine and Me3SiCl were added; mixt. was heated at 80-85°C for 8 h; cooled; volatiles removed (vac.); triturated with THF and hexane;
参考文献
Berget, Patrick E.; Schore, Neil E.
Organometallics, 2006 , vol. 25, # 2 p. 552 - 553