in hexane; cyclohexane
1-bromooctane (1 equiv.) and TMTH (2 equiv.) in hexane 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 (after quenching), NMR (before quenching);
参考文献
Reimann, Werner; Kuivila, Henry G.; Farah, Dan; Apoussidis, Theodorus
Organometallics, 1987 , vol. 6, p. 557 - 565
in tetrahydrofuran
TMTH (1.10 mmol) and 1-bromooctane (1.10 mmol) in THF cooled to 0°C under Ar, MeLi (1.10 mmol) in THF added, stirred for 15 min at room temp., hydrolyzed with water; H2 collected with gas measuring device, GC analysis of org. layer;
参考文献
Reimann, Werner; Kuivila, Henry G.; Farah, Dan; Apoussidis, Theodorus
Organometallics, 1987 , vol. 6, p. 557 - 565
in deuterated toluene
byproducts: (CF3)2PH; under exclusion of air and moisture in a closed NMR-tube, react. of theCr-complex with (CH3)3SnH in toluene-d8 at 0°C; not isolated, detected by NMR;
参考文献
Grobe, Joseph; Le Van, Duc
Zeitschrift fuer Naturforschung, Teil B: Anorganische Chemie, Organische Chemie, 1981 , vol. 36, p. 666 - 671
in deuterated toluene
under exclusion of air and moisture in a closed NMR-tube, react. of theMo-complex with (CH3)3SnH in toluene-d8 at 0°C; not isolated, detected by NMR;
参考文献
Grobe, Joseph; Le Van, Duc
Zeitschrift fuer Naturforschung, Teil B: Anorganische Chemie, Organische Chemie, 1981 , vol. 36, p. 666 - 671
