2,2-二甲基丙基次基膦合成路线 (共 36 条)
反应条件
in acetonitrile T=100°C; 5 h;
参考文献
Roesch, W.; Regitz, M.
Synthesis, 1987 , # 8 p. 689 - 693
反应条件
in toluene T=160 - 170°C; P=6000.5 Torr; 4 h;
参考文献
Julino, Markus; Slany, Michael; Bergstraesser, Uwe; Mercier, Francois; Mathey, Francois; Regitz, Manfred
Chemische Berichte, 1995 , vol. 128, # 10 p. 991 - 998
反应条件
in benzene t-butylphosphaacetylene was added to a mixture of dienes in benzene and heated in a closed vessel for 24 h at 120°C, filtration gave the polygermylene;; the solution was evapd. in vac., the is residue 2-t-butyl-4,5-dimethyl-λ(3)-phosphinine;;
参考文献
Andriamizaka, Jean-Dominique; Couret, Claude; Escudie, Jean; Laporterie, Andre; Manuel, Georges; Regitz, Manfred
Journal of Organometallic Chemistry, 1991 , vol. 419, # 1 p. 57 - 62
反应条件
in diethyl ether; pentane byproducts: C2H4; Ar atmosphere; dropwise addn. of PCC(CH3)3 (20.0 mmol) in ether/pentaneto a soln. of the Co complex (7.8 mmol) in ether/pentane at -30°C; mixt. was kept at -5°C for 1 h;; evapn.; residue was dissolved in pentane; filtration through Florisil; filtrate was cooled at -78°C for 12 h; removal of solvent; dryingat 1E-3 torr; elem. anal.;;
参考文献
Binger, Paul; Milczarek, Roman; Mynott, Richard; Krueger, Carl; Tsay, Yi-Hung; et al.
Chemische Berichte, 1988 , vol. 121, p. 637 - 646
反应条件
in diethyl ether; pentane Ar atmosphere, molar ratio complex/PC-t-Bu 1:1; chromy (Al2O3, toluene);
参考文献
Binger, Paul; Milczarek, Roman; Mynott, Richard; Krueger, Carl; Tsay, Yi-Hung; et al.
Chemische Berichte, 1988 , vol. 121, p. 637 - 646
反应条件
in toluene CpCo(C2H4)2 (9.4 mmol) and Me3SiCCSiMe3 (20 mmol) dissolved in toluene and heated to reflux, at this temp. t-BuCP (7 mmol) and Me3SiCCSiMe3 (10 mmol) in toluene added over 5 h, further stirred for 2 h; filtered through Florisil, evapd., chromd. (column, Kieselgel 60, hexane), CpCo((CSiMe3)4) isolated from 1st yellow eluate, next red eluate yielded CpCo(t-BuCP(CSiMe3)2) after evapn., last eluate contained CpCo((t-BuCP)2); elem. anal.;
参考文献
Binger, Paul; Milczarek, Roman; Mynott, Richard; Regitz, Manfred
Journal of Organometallic Chemistry, 1987 , vol. 323, p. C35 - C38
反应条件
in toluene T=110°C; 24 h; sealed tube;
参考文献
Tetrahedron Letters, , vol. 29, # 46 p. 5867 - 5870
反应条件
in diethyl ether Ar atmosphere, addn. of 2-butyne to complex in ether (-30°C), stirring, addn. of PC-t-Bu in ether (during 0.5 h, 0°C); volatiles removal (1E-2 Torr, darkness), chromy. (alumina, pentane), crystn. (cooling to -78°C), drying (1E-3 Torr); elem. anal.;
参考文献
Binger, Paul; Milczarek, Roman; Mynott, Richard; Krueger, Carl; Tsay, Yi-Hung; et al.
Chemische Berichte, 1988 , vol. 121, p. 637 - 646
反应条件
in toluene T=110°C; 24 h; sealed tube;
参考文献
Maerkl, G.; Dietl, S.; Ziegler, M. L.; Nuber, B.
Tetrahedron Letters, 1988 , vol. 29, # 46 p. 5867 - 5870
反应条件
selenium; triethylamine in toluene T=70°C; Cycloaddition; 24 h;
参考文献
Asmus, Sven M. F.; Bergstraesser, Uwe; Regitz, Manfred
Synthesis, 1999 , # 9 p. 1642 - 1650