双(五甲基环戊烯)二氯化钛合成路线 （共 24 条）
反应条件
in tetrahydrofuran addn. of (2-methyl-2-butene-1,4-diyl)magnesium soln. to a soln. of (C5Me5)2TiCl2 under Ar at -78°C; stirred ; stirred 2h at -45°C; allowed to warm up to room temp.; stirred 2; evapn.; extn. (hexane); centrifugation; concn.; cooled to -20°C; pptn.; repeated recrystn. (hexane, THF);
参考文献
Yamamoto, Hitoshi; Yasuda, Hajime; Tatsumi, Kazuyuki; Lee, Keonil; Nakamura, Akira; et. al.,
Organometallics, 1989 , vol. 8, p. 105 - 119
反应条件
in hexane addn. of hexane to organometallic in a dram vial; stirring; addn. of NMe2Oct*HCl suspn. in a dram vial; 1h; quickly evapg.; mechanism discussed; dissolving of dry residue (C6D6); detn. by NMR;
参考文献
Journal of Organometallic Chemistry, , vol. 414, # 1 p. 23 - 32
反应条件
PbCl2 in tetrahydrofuran; diethyl ether Ti-complex was mixed with Li-salt in THF, refluxed for 1 h, other Li-salt in Et2O was added, Et2O was distilled off, refluxed for 24 h, vol. wasreduced, PbCl2 was added under Ar, stirred for 2 h at 40°C under Ar; volatiles were evapd. under vac., extd. with hexane, crystd. from hexane;
参考文献
Journal of Organometallic Chemistry, , vol. 667, # 1-2 p. 154 - 166
反应条件
PbCl2 in tetrahydrofuran; diethyl ether Ti-complex was mixed with Li-salt in THF, refluxed for 1 h, other Li-salt in Et2O was added, Et2O was distilled off, refluxed for 24 h, vol. wasreduced, PbCl2 was added under Ar, stirred for 2 h at 40°C under Ar; volatiles were evapd. under vac., extd. with hexane, crystd. from hexane;
参考文献
Journal of Organometallic Chemistry, , vol. 667, # 1-2 p. 154 - 166
反应条件
in tetrahydrofuran T=0 - 20°C; Inert atmosphere;
参考文献
Organometallics, , vol. 31, # 24 p. 8544 - 8555
反应条件
in diethyl ether addn. of ether to organometallic in a dram vial; stirring; addn. of NMe2Oct*HCl suspn. in a dram vial; 1h; quickly evapg.; mechanism discussed; dissolving of dry residue (C6D6); detn. by NMR;
参考文献
Journal of Organometallic Chemistry, , vol. 414, # 1 p. 23 - 32
反应条件
in not given byproducts: dibenzyl ditelluride; in dark;
参考文献
Inorganic Chemistry, , vol. 34, p. 2499 - 2500
反应条件
in tetrahydrofuran byproducts: N-(2,2-diphenylvinyl)-4-methylaniline; N2-atmosphere; equimolar amts., stirring overnight;
参考文献
Organometallics, , vol. 16, # 24 p. 5283 - 5288
参考文献
Journal of the American Chemical Society, , vol. 117, # 29 p. 7814 - 7815
反应条件
in tetrahydrofuran byproducts: 1,4-bis(trimethylsilyl)buta-1,3-diyne; 70°C, 6 h;
参考文献
Journal of Organometallic Chemistry, , vol. 689, # 24 SPEC. ISS. p. 4592 - 4600
