2,8,9-三氧杂-5-氮杂-1-锗杂双环[3.3.3]十一烷-1-醇合成路线 (共 6 条)
反应条件
Et3N in ethanol; hexane; toluene
(N2); standard Schlenk technique; HSiCl3 was added via syringe to soln. of GeCl4 in hexane at 0°C; mixt. stirred for 30 min; Et3N was added dropwise; cold bath was removed; mixt. was stirred for 1 h; lower phase septd.; washed (hexane); toluene; added under N2; EtOH and Et3N added; mixt. stirred for 1 h; filtered; residue washed (toluene); filtrate and washings added to (EtO)3N in toluene; soln. stirred at room temp. for 16 h; filtered; residue washed (toluene; CH2Cl2); filtrate evapd. (vac);
参考文献
Faller; Kultyshev, Roman G.
Organometallics, 2003 , vol. 22, # 1 p. 199 - 202
反应条件
triethylamine in isopropyl alcohol; benzene
byproducts: Et3NHCl; addn. of Et3N to Ge-complex soln. (-5 to -10°C, stirring), warming to 20°C, triethanolamine addn., stirring (room temp., 16 h); filtration of ppt. and evapn. of filtrate (vac.); elem. anal.;
参考文献
Mironov, V. F.; Khromova, N. Yu.; Gar, T. K.
Journal of General Chemistry USSR (English Translation), 1981 , vol. 51, p. 795 - 796
Zhurnal Obshchei Khimii, 1981 , vol. 51, p. 954 - 955
反应条件
in neat (no solvent)
byproducts: Bu3SnCl; reactants mixed at -40°C;
参考文献
Karlov; Shutov; Akhmedov; Lorberth; Zaitseva
Russian Journal of General Chemistry, 2000 , vol. 70, # 6 p. 989 - 990
反应条件
in benzene
under dry N2; mixt. boiled for 35 min; cooled; triethanolamine hydriodide isolated; a mixt. pptd. by evapn. of filtrat;e; recrystd. from hexane and allylgermatrane isolated;
参考文献
Gar, T. K.; Khromova, N. Yu.; Tandura, S. N.; Mironov, V. F.
Journal of General Chemistry USSR (English Translation), 1983 , vol. 53, p. 1619 - 1626
Zhurnal Obshchei Khimii, 1983 , vol. 53, p. 1800 - 1807
反应条件
in diethyl ether
reacted (20°C, 4 d); elem. anal.;
参考文献
Gar, T. K.; Khromova, N. Yu.; Tandura, S. N.; Mironov, V. F.
Journal of General Chemistry USSR (English Translation), 1983 , vol. 53, p. 1619 - 1626
Zhurnal Obshchei Khimii, 1983 , vol. 53, p. 1800 - 1807
反应条件
in acetonitrile
byproducts: triethanolamine hydrobromide; under dry N2; mixt. boiled (81°C, 3 h); hot soln. decanted vac.-evapd. (20-100 mm, 30-35°C) until crystn. set in; ether added; solid 1-(triphenylmethyl)germatrane isolated; ppt. of chlorogermatrane obtained by evapn. of filtrate (40-50°C, 40mm); Ph3CH isolated from soln.; PMR;
参考文献
Gar, T. K.; Khromova, N. Yu.; Tandura, S. N.; Mironov, V. F.
Journal of General Chemistry USSR (English Translation), 1983 , vol. 53, p. 1619 - 1626
Zhurnal Obshchei Khimii, 1983 , vol. 53, p. 1800 - 1807