四氯双(四氢呋喃)合锆(IV)合成路线 (共 7 条)
反应条件
in toluene T=4 - 20°C; 1.25 h;
参考文献
WO2004/37839 A1, ;
Page/Page column 27 ;
反应条件
in dichloromethane-d2 byproducts: THF; at -80°C; not isolated, detected by NMR;
参考文献
Inorganic Chemistry, , vol. 29, p. 955 - 958
反应条件
in tetrahydrofuran under N2, Schlenk techniques; Zr complex dissolved in THF;
参考文献
Journal of the Chemical Society. Dalton Transactions, , # 19 p. 2844 - 2849
反应条件
1: n-amyl iodide; CpMgCl in tetrahydrofuran T=20 - 60°C; 4.08333 h; Inert atmosphere; 2: With n-butyllithium in hexanes; diethyl ether T=20°C; 0.666667 h; Inert atmosphere; 3: ZrCl4(tetrahydrofuran)2 in hexanes; diethyl ether T=20°C; 2.5 h; Inert atmosphere;
参考文献
UNIVATION TECHNOLOGIES, LLC; HARLAN, C., Jeff; CAO, Xianyi; RIX, Francis, C.
Patent: WO2011/136902 A1, 2011 ;
Location in patent: Page/Page column 13; 18 ;
反应条件
in tetrahydrofuran (N2); std. Schlenk technique; soln. of Na compd. (2 equiv.) in THF was slowly added to stirred suspn. of Zr compd. in THF at -78°C; warmed to room temp.; refluxed for 18 h; cooled; filtered; dried (vac.); sublimed (180°C, 0.1 Torr); elem.anal.;
参考文献
Organometallics, , vol. 28, # 6 p. 1838 - 1844
反应条件
in ethylene glycol dimethyl ether; toluene N2 atmosphere; addn. of soln. of org. compd. in DME to Zr-compd. in toluene, refluxing (1 h), stirring (12 h, room temp.); evapn., extn. (toluene), recrystn. (toluene);
参考文献
Zeitschrift fuer Naturforschung, B: Chemical Sciences, , vol. 48, # 7 p. 951 - 957
反应条件
n-butyllithium in tetrahydrofuran; hexane; toluene N2-atmosphere; dropwise addn. of BuLi (in hexane) to indene derivative (in THF) at -78°C, warming to room temp., stirring for 30 min, dropwise addn. to Zr-complex (in PhMe) over 2 h at 0°C, stirring (room temp., 2 h, pptn.); filtration, washing (THF/PhMe=1:2), drying (vac., overnight); elem. anal.;
参考文献
Lee, Gong Yeal; Xue, Ming; Kang, Myoung Soon; Kwon, Oh Chul; Yoon, Jin-San; Lee, Yoo-Su; Kim, Hoon Sik; Lee, Hyunjoo; Lee, Ik-Mo
Journal of Organometallic Chemistry, 1998 , vol. 558, # 1-2 p. 11 - 18