(三甲基硅基)甲基氯化镁合成路线 (共 130 条)
反应条件
NiCl2((PPh3)P)2 in ethylene glycol dimethyl ether; diethyl ether 6.5 h; Heating;
参考文献
Hevesi, Laszlo; Hermans, Bernard; Allard, Christophe
Tetrahedron Letters, 1994 , vol. 35, # 36 p. 6729 - 6730
参考文献
Chemical Communications, , # 3 p. 327 - 328
反应条件
in diethyl ether; hexane under N2 atm. slurry TaCl5 in hexane at -20°C was treated dropwise with Me3SiCH2MgCl in Et2O, solvent was removed in vacuo, residue was taken up in hexane at 0°C and filtered, PMe3 was added and heated to 50°C for 1 h; soln. was filtered, concd. and cooled to -20°C;
参考文献
Diminnie, Jonathan B.; Blanton, Jaime R.; Cai, Hu; Quisenberry, Keith T.; Xue, Ziling
Organometallics, 2001 , vol. 20, # 8 p. 1504 - 1514
反应条件
in diethyl ether 1 mol of complex was slowly added to an ether soln. of 2 mol RMgCl at -15°C, after 1 h the temp. was raised to room temp. (Ar atm.);; dioxane was added, ppt. was extd. with pentane; elem. anal.;;
参考文献
Journal of Organometallic Chemistry, , vol. 208, # 2 p. 169 - 182
反应条件
in diethyl ether byproducts: MgCl2; react. with Mg compd., then heating in Et2O;
参考文献
Legzdins, Peter; Phillips, Everett C.; Rettig, Steven J.; Sanchez, Luis; Trotter, James; Yee, Vivien C.
Organometallics, 1988 , vol. 7, p. 1877 - 1878
反应条件
1: trimethylsilyl-methylmagnesium chloride With zinc(II) iodide in diethyl ether Addition; 6 h; Heating; 2: 2-(2-phenylethyl)-1,3-dioxolane in benzene Grignard reaction; 8 h; Heating; Further stages.;
参考文献
Chiang, Chao-Cheng; Chen, Yu-Huei; Hsieh, Yu-Tsai; Luh, Tien-Yau
Journal of Organic Chemistry, 2000 , vol. 65, # 15 p. 4694 - 4697
反应条件
iron (III) acetylacetonate in tetrahydrofuran; 1-methyl-pyrrolidin-2-one; diethyl ether T=20°C; 0.0833333 h;
参考文献
ACADIA PHARMACEUTICALS INC.
Patent: WO2007/47776 A1, 2007 ;
Location in patent: Page/Page column 30; 31; 32; 42; 43 ;
反应条件
boron trifluoride diethyl etherate; copper (I) cyanide in diethyl ether under Ar; Mg compd. reacted with CuCN in ether (2:2, -45°C, 30-40min); BF3*OEt2 and Sn compd. reacted in ether (1:3, -80°C, 10 mi n or -45°C, 40 min); soln. of Sn compd. cannulated on soln. of Mg-Cu compd. (-80 or -40°C, 1 h); hydrolyzed with NaHCO3; chromd. (silica gel, MeCN-CH2Cl2 80:20); detd. by (1H) NMR spectra;
参考文献
Fliegel, Florian; Beaudet, Isabelle; Watrelot-Bourdeau, Sandrine; Cornet, Nicolas; Quintard, Jean-Paul
Journal of Organometallic Chemistry, 2005 , vol. 690, # 3 p. 659 - 673
反应条件
in diethyl ether 16 h; cooling;
参考文献
Paquet, Valerie; Lebel, Helene
Synthesis, 2005 , # 11 art. no. M07604SS, p. 1901 - 1905
参考文献
Fessenden; Coon
Journal of medicinal chemistry, 1965 , vol. 8, # 5 p. 604 - 608