三(1,2-苯二醇酸根-O,O')锗酸二钾合成路线 (共 20 条)
反应条件
2,3-butanediol in methanol (N2); added a soln. of CH3OK and than a soln. of catechol and 2,3-butanediol to suspn. of GeO2; refluxed for 2 h; evapd.; washed with ether; dried in vacuo; IR;
参考文献
Cerveau, G.; Chuit, C.; Corriu, J. P.; Reye, C.
Organometallics, 1991 , vol. 10, p. 1510 - 1515
反应条件
in methanol (N2); added a soln. of catechol to soln. of Ge-compound; stirred for 2 h; pptd.; evapd.; washed with ether; dried in vacuo;
参考文献
Cerveau, G.; Chuit, C.; Corriu, J. P.; Reye, C.
Organometallics, 1991 , vol. 10, p. 1510 - 1515
反应条件
magnesium; ethylene dibromide in diethyl ether (N2); added dropwise a mixture of 1,2-dibromoethane and CH2CHCH2Br to a ice-cooled suspn. of Mg over 6 h; added dropwise to a suspn. of Ge-compound at 0°C under stirring over 1 h; hydrolyzed; filtered; evapd.; distd.;
参考文献
Cerveau, G.; Chuit, C.; Corriu, J. P.; Reye, C.
Organometallics, 1991 , vol. 10, p. 1510 - 1515
反应条件
in tetrahydrofuran (N2); added dropwise a soln. of CH2CHCH2MgBr to a suspn. of Ge-compound; stirred for 1 h at room temp.; hydrolyzed; extracted with ether; washed with water; dried over MgSO4; evapd.;
参考文献
Cerveau, G.; Chuit, C.; Corriu, J. P.; Reye, C.
Organometallics, 1991 , vol. 10, p. 1510 - 1515
反应条件
methyl-magnesium iodide in further solvent(s) (N2); suspended Ge-compound in n-Bu2O; added dropwise a soln. of CH3MgI at room temp.; distd.;
参考文献
Cerveau, G.; Chuit, C.; Corriu, J. P.; Reye, C.
Organometallics, 1991 , vol. 10, p. 1510 - 1515
反应条件
bis(cyclopentadienyl)titanium dichloride in diethyl ether dropwise addn. of n-BuMgBr at room temp. to suspn. of Ge comp. and Cp2TiCl2 in Et2O under N2, mixt. is heated to reflux for 4 h; mixt. is hydrolized with aq. HCl, extn. (ether), washing (H2O, NaOH, brine), drying (MgSO4), evapn., distn.;
参考文献
Cerveau, G.; Chuit, C.; Corriu, R. J. P.; Reye, C.
Organometallics, 1988 , vol. 7, p. 786 - 787
反应条件
magnesium in tetrahydrofuran (N2); heated a suspn. of Mg and Ge-compound under stirring to 50°C; added dropwise a soln. of bromo benzene over 1.5 h; refluxed for 2 h; cooled; added ether; hydrolyzed; pptd.; filtered; washed with water, acetone and ether; dried; extracted with ether; washed with water; evapd.; recrystd. from toluene; GC;
参考文献
Cerveau, G.; Chuit, C.; Corriu, J. P.; Reye, C.
Organometallics, 1991 , vol. 10, p. 1510 - 1515
反应条件
magnesium; ethylene dibromide in diethyl ether (N2); added dropwise a mixture of 1,2-dibromoethane and C6H5Br to a ice-cooled suspn. of Mg over 6 h; added to a suspn. of Ge-compound at 0°C under stirring over 1 h; added LiAlH4; refluxed for 2 h; hydrolyzed; filtered; extracted with ether; crystd. from methanol;
参考文献
Cerveau, G.; Chuit, C.; Corriu, J. P.; Reye, C.
Organometallics, 1991 , vol. 10, p. 1510 - 1515
反应条件
magnesium; ethylene dibromide; phenyl-magnesium bromide in diethyl ether (N2); added dropwise a soln. of 1,2-dibromoethane to suspn. of Mg; stirred for 2,5 h; added a suspn. of Ge-compound and a soln. of C6H5MgBr over a period of 45 min at 20°C; stirred for 1 h at 20°C; added LiAlH4; refluxed for 1 h; cooled; added ethane; evapd.; distd.; GC;
参考文献
Cerveau, G.; Chuit, C.; Corriu, J. P.; Reye, C.
Organometallics, 1991 , vol. 10, p. 1510 - 1515
反应条件
magnesium in tetrahydrofuran (N2); heated a suspn. of Mg and Ge-compound under stirring to 50-55°C; added dropwise a soln. of ethyl bromide; refluxed under stirring for 2 h; cooled; added ether; evapd.; distd.;
参考文献
Cerveau, G.; Chuit, C.; Corriu, J. P.; Reye, C.
Organometallics, 1991 , vol. 10, p. 1510 - 1515