in pentane byproducts: SiMe4; The reagents in benzene were combined in a reaction tube, evacuated and heated at 55°C for 7 d;; mixt. was cooled to -78°C, filtered, washed with benzene, recrystd. from pentane at -78°C; elem. anal.;;
参考文献
Journal of Organometallic Chemistry, , vol. 325, p. 69 - 82
in benzene The mixt. of reagents in benzene was heated at 160-165°C for 3 weeks in a sealed tube;; not sepd., detected by NMR 13P spectra;;
参考文献
Beachley, O. T.; Kopasz, John P.; Zhang, Hongming; Hunter, William E.; Atwood, Jerry L.
Journal of Organometallic Chemistry, 1987 , vol. 325, p. 69 - 82
2,2'-azo-bisisobutyronitrile in neat (no solvent) under N2 atm. mixt. (OC)5WPPh(CH=CH2)2, PPh2H and 2,2'-azobis(isobutyronitrile) heated for 24 h at 75°C, excess PhP(CH=CH2)2 removed under high vac. after which (OC)5WPPh2H and AIBN added and mixt. heated for24 h at 75°C; oil dissolved in min. CH2Cl2 and CH3OH and refrigerated at 6°C;
参考文献
Keiter, Richard L.; Brodack, James W.; Borger, Rodney D.; Cary, Lew W.
Inorganic Chemistry, 1982 , vol. 21, p. 1256 - 1259
Khachatryan, R. A.; Sayadyan, S. V.; Grigoryan, N. Yu.; Indzhikyan, M. G.
J. Gen. Chem. USSR (Engl. Transl.), 1988 , vol. 58, # 11 p. 2472 - 2478,2197 - 2203
1: bis-diphenylphosphine With potassium tert-butylate in tetrahydrofuran T=20°C; 0.25 h; 2: 2-dimethylamino-1-chloro-ethane hydrochloride in tetrahydrofuran T=75°C; 16 h;
参考文献
Arakawa, Machiko; Suzuki, Noriyuki; Kishi, Shinobu; Hasegawa, Miki; Satoh, Keiichi; Horn, Ernst; Fukuda, Yutaka
Bulletin of the Chemical Society of Japan, 2008 , vol. 81, # 1 p. 127 - 135