in hexane; cyclohexane to 1-iodoheptane (1 mmol) and TMTH (1 mmol) in hexane at 0°C added LDA (1 mmol, in cyclohexane) under Ar, stirred for 20 min, quenched; analyzed by GLPC;
n-butyllithium in hexane 1-chloroheptane (1 equiv.) and TMTH (1 equiv.) in hexane cooled to 0°C under Ar, n-BuLi (1 equiv., 2.40 M in hexane) added, stirred for 4 h, quenched with water; analyzed by GC;
n-butyllithium in hexane n-BuLi (0.81 mmol, 0.70 M soln. in hexane) added to mixt. of 1-bromoheptane (0.81 mmol), 3-bromo-3-ethylpentane(0.81 mmol), and TMTH (0.81 mmol) in hexane under Ar, after 15 min of stirring at 0°C quenched with water; analyzed by GC;
in diethyl ether; cyclohexane 1-chloroheptane (1 equiv.) and TMTH (2 equiv.) in Et2O cooled to 0°C under Ar, LDA (1 equiv., 1.6 M soln. in cyclohexane) dropped in, stirred for 20-25 min at room temp., quenched with water; analyzed by GC;
in not given byproducts: Hg, iso-C4H10; reaction for 12 h at 20°C;;
参考文献
Blaukat, U.; Neumann, W. P.
Journal of Organometallic Chemistry, 1973 , vol. 63, p. 27 - 39
Full Text Show Details
Gmelin Handbook: Sn: Org.Verb.4, 1.2.1.1.1.4.6, page 17 - 18
in benzene byproducts: (CH3)3COH; at 50°C in 20 h;;
参考文献
Christen, U.; Neumann, W. P.
Chemische Berichte, 1973 , vol. 106, p. 421 - 434
Full Text Show Details
Gmelin Handbook: Sn: Org.Verb.4, 1.2.1.1.1.4.5, page 16 - 16
n-butyllithium in hexane 3-bromo-3-ethylpentane (1 equiv.) and TMTH (1 equiv.) in hexane cooled to 0°C under Ar, n-BuLi (1 equiv., 2.40 M in hexane) added, stirred for 15 min, quenched with water; analyzed by GC;
n-butyllithium in hexane n-BuLi (0.81 mmol, 0.70 M soln. in hexane) added to mixt. of 1-bromoheptane (0.81 mmol), 3-bromo-3-ethylpentane(0.81 mmol), and TMTH (0.81 mmol) in hexane under Ar, after 15 min of stirring at 0°C quenched with water; analyzed by GC;
in neat (no solvent) condensing of equimolar amts. of tinhydride and SiClHBr2 (trace of SiCl2HBr present) into cold finger, reaction at room temp. (30 min); further products; not isolated; IR spectroscopy;
参考文献
D'Errico, John J.; Sharp, Kenneth G.
Inorganic Chemistry, 1989 , vol. 28, p. 2177 - 2180
