2,3-二甲基-1,3-丁二烯合成路线 (共 777 条)
反应条件
in toluene
heating a mixt. of Ge3Mes6 and 2,3-dimethylbutadiene in toluene to 100°C for 4 h or refluxing in benzene for 15 h under an atmosphere of argon; evapn. of the solvent, preparative TLC, elem. anal.;
参考文献
Baines, Kim M.; Cooke, Jeffrey A.; Dixon, Craig E.; Liu, Hui Wen; Netherton, Matthew R.
Organometallics, 1994 , vol. 13, p. 631 - 634
反应条件
in cyclohexane
Irradiation (UV/VIS); irradiation with a low-pressure mercury lamp for 4 h at room temp.; preparative TLC (silica gel, benzene/hexane);
参考文献
Tsumuraya, Takeshi; Sato, Sadao; Ando, Wataru
Organometallics, 1988 , vol. 7, p. 2015 - 2019
反应条件
in cyclohexane
Irradiation (UV/VIS); irradiating cyclohexane soln. of 3-alkylidenethiagermirane and 2,3-dimethyl-1,3-butadiene (low-pressure mercury lamp, 6 h, room temp.); preparative TLC (silica gel, benzene/hexane 1:3);
参考文献
Ando, Wataru; Tsumuraya, Takeshi
Organometallics, 1989 , vol. 8, p. 1467 - 1472
反应条件
in benzene
pyrolysis at 470°C under flowing N2; preparative TLC (silica gel, benzene/hexane); elem. anal.;
参考文献
Tsumuraya, Takeshi; Sato, Sadao; Ando, Wataru
Organometallics, 1988 , vol. 7, p. 2015 - 2019
反应条件
in cyclohexane
Irradiation (UV/VIS); under Ar; photolysis at room temp.; 5h; sepn. by preparative HPLC;
参考文献
Tsumuraya, Takeshi; Sadao, Sato; Ando, Wataru
Organometallics, 1989 , vol. 8, p. 161 - 167
反应条件
in benzene
by reflux of a soln. of (Ge(Mes)2)3 and 2,3-dimethylbuta-1,3-diene in benzene for 10 h a mixture of the 1,2-digermacyclohex-4-ene and germacyclopent3-ene is obtained; elem. anal.;
参考文献
Ando, Wataru; Tsumuraya, Takeshi
Journal of the Chemical Society, Chemical Communications, 1989 , # 12 p. 770 - 771
反应条件
in benzene-d6
pyrolyzed at 495°C under flowing N2; Sepn. by preparative TLC;
参考文献
Tsumuraya, Takeshi; Sadao, Sato; Ando, Wataru
Organometallics, 1989 , vol. 8, p. 161 - 167
反应条件
triethylamine in benzene
byproducts: (C2H5)3NHCl; Et3N adding in excess to germane soln. in benzene, stirring at ambient temp., Et3NHCl filtering off, ligand adding, heating for 6 h at 130°C; identified by NMR spectrum;
参考文献
Riviere, P.; Castel, A.; Satge, J.
Journal of Organometallic Chemistry, 1982 , vol. 232, # 2 p. 123 - 136
反应条件
in benzene
flow copyrolysis of benzene soln. of 3-alkylidenethiagermirane and 2,3-dimethyl-1,3-butadiene (500°C, nitrogen flow 10 ml/min, trapping pyrolysate in a receiver cooled by dry ice-MeOH); preparative TLC (silica gel, benzene/hexane 1:3);
参考文献
Ando, Wataru; Tsumuraya, Takeshi
Organometallics, 1989 , vol. 8, p. 1467 - 1472
反应条件
in not given
trapped by 2,3-dimethylbutadiene (Mes2Ge/C4H4(CH3)2=1/30); column chromy., mass spectra, NMR;
参考文献
Egorov, M. P.; Kolesnikov, S. P.; Nefedov, O. M.; Krebs, A.
Journal of Organometallic Chemistry, 1989 , vol. 375, p. C5 - C8