in tetrahydrofuran soln. of alkene in THF was added to soln. of Re complex in THF at room temp.; reacted at room temp. for 30 min; THF removed; Et2O added; filtered through Celite; 18-crown-6 ether and dioxane consecutively added; filtered; residue dissolved in Et2O; dioxaneadded; pptd.; mother liquor chromd. (silica gel, ether, petroleum ether /CH2Cl2, 4/1);
参考文献
Sazonov; Artamkina; Lyssenko; Beletskaya
Journal of Organometallic Chemistry, 2006 , vol. 691, # 11 p. 2346 - 2357
in tetrahydrofuran byproducts: Te; N2-atmosphere; stirring Re-complex, Na and crown ether, slow addn. to TeCl4 at -20°C), then at room temp.; sepn. by THF-hexane;
1: With [bis(acetoxy)iodo]benzene; copper(II) bis(trifluoromethanesulfonate) in dichloromethane T=40°C; 4 h; 2: With sodium tetrahydroborate in tetrahydrofuran T=25°C; Further stages.;