(2,3,4,5,6-五氟苯基)-三(苯基)锡烷合成路线 (共 18 条)
反应条件
magnesium in diethyl ether
Ar-atmosphere; addn. of excess of Grignard reagent (prepd. from Mg and C6H5Br) to Sn-compd. at 0°C, stirring (room temp., 2 h); filtration (celite), chromy. (SiO2, hexane);
参考文献
Chen, Jian-Xie; Sakamoto, Katsumasa; Orita, Akihiro; Otera, Junzo
Journal of Organometallic Chemistry, 1999 , vol. 574, # 1 p. 58 - 65
反应条件
in diethyl ether
refluxing, 3 days;;
参考文献
Gmelin Handbook: Sn: Org.Verb.2, 1.1.2.15.7, page 408 - 418
反应条件
sulfuric acid in tetrahydrofuran
byproducts: YbCl2; Sn-complex was added under N2 to soln. of Yb-complex in THF at 0°C for 2.5 h, solvent was removed under vac., residue was hydrolysed with H2SO4; organic layer was washed with aq. NaHCO3, dried, evapd., recrystd. from aq. EtOH;
参考文献
Deacon, Glen B.; Mackinnon, Peter I.; Tuong, Tran D.
Australian Journal of Chemistry, 1983 , vol. 36, p. 43 - 54
反应条件
in diethyl ether
refluxing;;
参考文献
Gmelin Handbook: F: PerFHalOrg.4, 2.2.4, page 68 - 115
反应条件
in tetrahydrofuran
Ar atmosphere; addn. of Ph3SnCl in THF to soln. of C6F5YbBr (20°C), stirring (1 h, 20°C); addn. of water, extn. (ether), drying of extract (over MgSO4);
参考文献
Rybakova, L. F.; Syutkina, O. P.; Petrov, E. S.; Shifrina, R. R.; Beletskaya, L. P.
Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), 1984 , vol. 33, # 6 p. 1301 - 1303
Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, 1984 , # 6 p. 1413 - 1415
反应条件
in tetrahydrofuran
at 10°C; the C6F5YbBr (in situ) is treated with (C6H5)3SnCl; warmed to 25°C, after hydrolysis acidified with HCl, septd., extractd. with ether, dried over Na2SO4;; TLC;
参考文献
Syutkina, O. P.; Rybakova, L.F.; Petrov, E. S.; Beletskaya, I. P.
Journal of Organometallic Chemistry, 1985 , vol. 280, p. C67 - C69
反应条件
in tetrahydrofuran
at 20°C; C6F5CeI (in situ) is treated with (C6H5)3SnCl; warmed to 25°C, after hydrolysis acidified with HCl, septd., extractd. byether, dried over Na2SO4; TLC;
参考文献
Syutkina, O. P.; Rybakova, L.F.; Petrov, E. S.; Beletskaya, I. P.
Journal of Organometallic Chemistry, 1985 , vol. 280, p. C67 - C69
反应条件
[Ni0(1,5-cyclooctadiene)2]; MeNC5H4NiPr in benzene-d6
T=20°C; 2 h; Inert atmosphere;
参考文献
Doster, Meghan E.; Johnson, Samuel A.
Organometallics, 2013 , vol. 32, # 15 p. 4174 - 4184
反应条件
in tetrahydrofuran
Ar atmosphere; addn. of C6HF5 in THF to soln. of MeYbI (20°C), stirring (40 min), addn. of Ph3SnCl in THF, stirring (1 h); addn. of water, extn. (ether), drying of extract (over MgSO4);
参考文献
Rybakova, L. F.; Syutkina, O. P.; Petrov, E. S.; Shifrina, R. R.; Beletskaya, L. P.
Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), 1984 , vol. 33, # 6 p. 1301 - 1303
Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, 1984 , # 6 p. 1413 - 1415
反应条件
1: I2; HCl
2: diethyl ether
View Scheme
参考文献
Gmelin Handbook: Sn: Org.Verb.2, 1.1.2.15.7, page 408 - 418