2-(三甲基甲锡烷基)吡啶合成路线 (共 46 条)
反应条件
n-butyllithium in tetrahydrofuran; diethyl ether; hexane under N2, n-BuLi in hexane cooled to -78°C, dild. with Et2O, ethereal soln. of heterocycle added dropwise with stirring, stirred for a while, after addn. of soln. of Me3SnCl in THF allowed to warm to room temp.; concd. in vac., methylcyclohexane added, filtered, fractionally distd.;elem. anal.;
参考文献
Jutzi, Peter; Gilge, Ullrich
Journal of Organometallic Chemistry, 1983 , vol. 246, # 2 p. 163 - 168
反应条件
methyl iodide in ammonia Irradiation (UV/VIS); condensation of sodium-dried ammonia into round-bottomed Pyrex flask, addn. of Me3SnCl and Na, addn. of C5H4NNMe3I; irradn. with stirring for 4 h, quenching by addn. of MeI in excess; evapn. of ammonia, treatment with water, extn. with ether;
参考文献
Chopa, Alicia B.; Lockhart, Maria T.; Silbestri, Gustavo
Organometallics, 2001 , vol. 20, # 15 p. 3358 - 3360
反应条件
sodium in ammonia Irradiation (UV/VIS); (CH3)3SnCl was dissolved in ammonia, Na metal was added until a blue color persisted for 5 min, when the blue color dissapeared, phosphate esterwas added, the mixt. was UV-irradiated with stirring for 4 h; excess of CH3I was added, NH3 was evapd., the residue was treated with water, extd. with ether, washed with aq. satd. soln. of NaCl, dried over MgSO4, recrystd. in ethanol;
参考文献
Chopa, Alicia B.; Lockhart, Maria T.; Dorn, Viviana B.
Organometallics, 2002 , vol. 21, # 7 p. 1425 - 1429
反应条件
in ammonia NH3 (liquid); Irradiation (UV/VIS); (inert atm.); addn. of 4.4 equiv. of sodium to soln. of 2.2 equiv. of tin compd. in liquid ammonia, addn. of 1 equiv. of pyridine deriv., stirring with irradiation for 30 min; quenching with methyl iodide, adn. of diethyl ether, evapn. of ammonia, treating with water, extn. (diethyl ether), washing with water and brine, drying over MgSO4, filtration, evapn., recrystn. (ethanol), NMR and MS;
参考文献
Silbestri, Gustavo F.; Lo Fiego, Marcos J.; Lockhart, Maria T.; Chopa, Alicia B.
Journal of Organometallic Chemistry, 2010 , vol. 695, # 24 p. 2578 - 2585
反应条件
in ammonia NH3 (liquid); Irradiation (UV/VIS); (inert atm.); addn. of 4.4 equiv. of sodium to soln. of 2.2 equiv. of tin compd. in liquid ammonia, addn. of 1 equiv. of pyridine deriv., stirring with irradiation for 20 min; quenching with methyl iodide, adn. of diethyl ether, evapn. of ammonia, treating with water, extn. (diethyl ether), washing with water and brine, drying over MgSO4, filtration, evapn., distd in vac., NMR and MS;
参考文献
Silbestri, Gustavo F.; Lo Fiego, Marcos J.; Lockhart, Maria T.; Chopa, Alicia B.
Journal of Organometallic Chemistry, 2010 , vol. 695, # 24 p. 2578 - 2585
反应条件
C6H4(NO2)2 in ammonia NH3 (liquid); (inert atm.); addn. of 4.4 equiv. of sodium to soln. of 2.2 equiv. of tin compd. in liquid ammonia, addn. of 1 equiv. of pyridine deriv. and p-dinitrobenzene, stirring for 60 min in dark;
参考文献
Journal of Organometallic Chemistry, , vol. 695, # 24 p. 2578 - 2585
反应条件
C6H4(NO2)2 in ammonia byproducts: C5H4N(OPO(OCH2CH3)2); NH3 (liquid); (inert atm.); addn. of 4.4 equiv. of sodium to soln. of 2 equiv. of tin compd. in liquid ammonia, addn. of 1 equiv. of pyridine deriv. and p-dinitrobenzene, stirring for 30 min; quenching, GC/MS anal.;
参考文献
Journal of Organometallic Chemistry, , vol. 695, # 24 p. 2578 - 2585
反应条件
in ammonia NH3 (liquid); Irradiation (UV/VIS); (inert atm.); addn. of 2.2 equiv. of sodium to soln. of 1 equiv. of tin compd. in liquid ammonia, addn. of 1 equiv. of pyridine deriv. and p-dinitrobenzene, stirring with irradiation for 30 min; quenching, GC/MS anal.;
参考文献
Journal of Organometallic Chemistry, , vol. 695, # 24 p. 2578 - 2585
反应条件
in ammonia NH3 (liquid); Irradiation (UV/VIS); (inert atm.); addn. of sodium to soln. of 2.2 or 5 equiv. of tin compd. in liquid ammonia, addn. of 1 equiv. of pyridine deriv., stirring with irradiation for 180 min; quenching with methyl iodide, adn. of diethyl ether, evapn. of ammonia, treating with water, extn. (diethyl ether), washing with water and brine, drying over MgSO4, filtration, evapn., distd in vac., NMR and MS;
参考文献
Journal of Organometallic Chemistry, , vol. 695, # 24 p. 2578 - 2585
反应条件
in ammonia NH3 (liquid); (inert atm.); addn. of 4.4 equiv. of sodium to soln. of 2 equiv. of tin compd. in liquid ammonia, addn. of 1 equiv. of pyridine deriv., stirringfor 180 min in dark; quenching, GC/MS anal.;
参考文献
Journal of Organometallic Chemistry, , vol. 695, # 24 p. 2578 - 2585