CH3MgBr in diethyl ether; benzene byproducts: tetraphenylnaphthalene; Norbornadiene-compound and Me2GeBr2 are heated at 75°C for 4 h in benzene, reaction mixture is methylated with MeMgBr in Et2O at 0°C with stirring for 0.5 h then stirring for 1 h at room temp. (Ar).; addn. of H2O and NH4Cl at 0°C, sepn., extn. of aq. phase (Et2O), removal of solvent, GC-MS anal. demonstrates the formation of Me8Ge3 and Me10Ge4 as the methylation products in ratio 1:1;
参考文献
Koecher, Juergen; Lehnig, Manfred; Neumann, Wilhelm P.
Organometallics, 1988 , vol. 7, p. 1201 - 1207
CH3MgBr in diethyl ether Methylation of reaction mixture with MeMgBr in Et2O at 0°C with stirring for 0.5 h, then stirring of the mixture at room temp. for 1 h under Ar.; addn. of H2O and NH4Cl, sepn. of phases, extn. of aq. phase (Et2O), removal of solvent, pptn. of tetraphenylnaphthalene (pentane), investigation of crude products by GC-MS anal.;
参考文献
Koecher, Juergen; Lehnig, Manfred; Neumann, Wilhelm P.
Organometallics, 1988 , vol. 7, p. 1201 - 1207
CH3MgBr in diethyl ether Methylation of reaction mixture with MeMgBr in Et2O at 0°C with stirring for 0.5 h, then stirring of the mixture at room temp. for 1 h under Ar.; addn. of H2O and NH4Cl, sepn. of phases, extn. of aq. phase (Et2O), removal of solvent, pptn. of tetraphenylnaphthalene (pentane), investigation of crude products by GC-MS anal.;
参考文献
Koecher, Juergen; Lehnig, Manfred; Neumann, Wilhelm P.
Organometallics, 1988 , vol. 7, p. 1201 - 1207
CH3MgBr in diethyl ether Methylation of reaction mixture with MeMgBr in Et2O at 0°C with stirring for 0.5 h, then stirring of the mixture at room temp. for 1 h under Ar.; addn. of H2O and NH4Cl, sepn. of phases, extn. of aq. phase (Et2O), removal of solvent, pptn. of tetraphenylnaphthalene (pentane), investigation of crude products by GC-MS anal.;
参考文献
Koecher, Juergen; Lehnig, Manfred; Neumann, Wilhelm P.
Organometallics, 1988 , vol. 7, p. 1201 - 1207
methylphosphonous dichloride in neat (no solvent) room temp., 20 d; not isolated, equilibrium concns. with educts detd. by (1)H-NMR spectroscopy; equilibrium ratio of products depending on ratio of educts;
参考文献
Moedritzer
Inorganica Chimica Acta, 1976 , vol. 17, p. 205,206,207,209
methylphosphonothioic dichloride in neat (no solvent) 120°C, 13 d; not isolated, equilibrium concns. with educts detd. by (1)H-NMR spectroscopy; equilibrium ratio of products depending on ratio of educts;
参考文献
Moedritzer
Inorganica Chimica Acta, 1976 , vol. 17, p. 205,206,207,209
methylphosphonyl dichloride in neat (no solvent) 120°C, 25 d; not isolated, equilibrium concns. with educts detd. by (1)H-NMR spectroscopy; equilibrium ratio of products depending on ratio of educts;
参考文献
Moedritzer
Inorganica Chimica Acta, 1976 , vol. 17, p. 205,206,207,209