in neat (no solvent, gas phase) Irradiation (UV/VIS); SnHMe3 at pressure 0.29 mTorr in 100 Torr of N2 photolyzed at 193 nm; 25-100 photolysis laser shots of photolysis pulce energy 40-50 mJ/pulse;
参考文献
Journal of the American Chemical Society, , vol. 124, # 25 p. 7555 - 7562
Burg, A. B.; Spielman, J. R.
Journal of the American Chemical Society, 1961 , vol. 83, p. 2667 - 2668
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Gmelin Handbook: Sn: Org.Verb.4, 1.2.1.1.1.4.5, page 16 - 16
in diethyl ether; cyclohexane Me3SiCH2Cl (5 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 hexane; cyclohexane to soln. of 1-iodoheptane (1.0 mmol) and TMTH (1.0 mmol) in hexane at 0°C added LDA (1.0 mmol, 1.6 M soln. in cyclohexane) under Ar, react. time 10 min; analyzed by GLPC;
in diethyl ether; cyclohexane to 6-bromo-1-hexene (1.04 mmol) and 2 equiv. of Me3SnH in Et2O at 0°C added LDA (1.04 mmol, in cyclohexane) under Ar, react. time 20 min, quenched with water; analyzed by GLPC;
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;
in hexane; cyclohexane to p-bromotoluene (1.02 mmol) and Me3SnH (2.04 mmol) in hexane at 0°C added LDA (1 mmol, in cyclohexane) under Ar, react. time 20 min, quenched with water; analyzed by GLPC;
in diethyl ether; cyclohexane to 1-bromoadamantane (1 mmol) and TMTH (1 mmol) in Et2O at 0°C added LDA (1 mmol, in cyclohexane) under Ar, stirred for 20 min, quenched; analyzed by GLPC;