hydrogen bromide in not given Under stirring a strong stream of hydrogenhalogenide is bubbled for 3-10 min through the cooled (-50-0°C) soln. of phosphine complex (inert atmosphere).; Solvent is evapd. at room temp. in vac., residue is digested with pentane, dialkylamminhydrohalogenide is filtered off, filtrate is dried to dryness in vac., recrystn. from pentane (-78°C), not purely isolated.;
参考文献
Diemert, K.; Kuchen, W.; Lorenzen, D.
Journal of Organometallic Chemistry, 1989 , vol. 378, p. 17 - 32
hydrogenchloride in diethylamine (dry Ar); heated in sealed ampul for 80 h at 100°C; ppt. Et2NH*HBr filtered; filtrate treated MeOH; fraction vac. distn.; treated ether soln. HCl; sepd.; filtrate distn.; elem. anal.;
参考文献
Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), , vol. 29, # 5 p. 813 - 820
Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, , # 5 p. 1106 - 1113
in neat (no solvent) (dry Ar); sealed ampul; heated for 40 h at 100°C; ppt. Et2NH2Br filtered; washed (Et2NH); filtrate heated for 100 h; additional isolatedEt2NH2Br; filtrate distn.; elem. anal.;
参考文献
Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), , vol. 29, # 5 p. 813 - 820
Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, , # 5 p. 1106 - 1113
→
反应条件
in toluene Kinetics; N2 atmosphere, 40.0+/-0.5°C; GLC;
参考文献
Bulletin of the Chemical Society of Japan, , vol. 61, p. 1251 - 1258