iodine; methyl iodide in ethanol Sonication; N2, CH3I, I2 and Al introduced in a condenser with C2H5OH at -20°C, ultrasonic acceleration at room temp. for 2 h, Et3Al (ratio MeI/Et3Al = 0.75) dropped into soln. within 10 min, sonicated for 30 min; distilled (vac.);
参考文献
Yang, Paw-Hwa; Liou, Kou-Fu; Lin, Yih-Tsung
Journal of Organometallic Chemistry, 1986 , vol. 307, p. 273 - 278
in neat (no solvent) under Ar atm. excess Me2AlH and di(tert-butyl)butadiyne were stirred at 100°C for 1.5 h; react. mixt. was cooled to room temp., volatiles were removed in vacuo, residue was dissolved in n-pentane and cooled to -15°C;
参考文献
Uhl, Werner; Vinogradov, Andrej; Grimme, Stefan
Journal of the American Chemical Society, 2007 , vol. 129, # 36 p. 11259 - 11264
iodine; methyl iodide in ethanol Sonication; N2, CH3I, I2 and Al introduced in a condenser with C2H5OH at -20°C, ultrasonic acceleration at room temp. for 2 h, Et3Al (ratio MeI/Et3Al = 3.00) dropped into soln. within 10 min, sonicated for 30 min; distilled (vac.);
参考文献
Journal of Organometallic Chemistry, , vol. 307, p. 273 - 278
iodine; methyl iodide in ethanol Sonication; N2; CH3I, I2 and Al introduced in a condenser with C2H5OH at -20°C, ultrasonic acceleration at room temp. for 2 h, Et3Al (ratio MeI/Et3Al = 1.50) dropped into soln. within 10 min, sonication for 30 min; distilled (vac.);
参考文献
Journal of Organometallic Chemistry, , vol. 307, p. 273 - 278
Journal of the American Chemical Society, , vol. 68, p. 2204
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反应条件
in hexane; toluene byproducts: CH4; in a glovebox, Y-contg. compd. (0.50 mmol) was dissolved in hexane, and a toluene suspn. of carboxylic acid (0.50 mmol) was slowly added; stirring at ambient temp. for 18 h; the solvent was removed in vac.; extn. in toluene; the complex was washed with hexane and dried for several hours; elem. anal.;
in hexane byproducts: CH4; Schlenk technique; diene (1 equiv.) in hexane was added with stirring tosoln. of Y complex in hexane; mixt. was stirred for 5 min; solvent removed (vac.); dried (vac.); elem. anal.;
参考文献
Dietrich, H. Martin; Zapilko, Clemens; Herdtweck, Eberhardt; Anwander, Reiner
Organometallics, 2005 , vol. 24, # 23 p. 5767 - 5771
iodine; methyl iodide in ethanol Sonication; N2, CH3I, I2 and Al introduced in a condenser with C2H5OH at -20°C, ultrasonic acceleration at room temp. for 2 h, Et3Al (ratio MeI/Et3Al = 12.00) dropped into soln. within 10 min, sonicated for 30 min; distilled (vac.);
参考文献
Journal of Organometallic Chemistry, , vol. 307, p. 273 - 278
→
反应条件
in hexane; toluene byproducts: CH4; in a glovebox, Nd-contg. compd. (0.40 mmol) was dissolved in hexane, anda toluene suspn. of carboxylic acid (0.40 mmol) was slowly added; stirr ing at ambient temp. for 18 h; the solvent was removed in vac.; extn. in toluene; the complex was washed with hexane and dried for several hours; purifn. by crystn.; elem. anal.;
