in benzene-d6 under Ar, standard vac. line techniques; In compd. and ClP(i-Pr)2 (molarratio 1.07:1) combined under vac. in benzene-d6; stirred for 18 h; comb ined with benzene-d6 soln. of K-In compd. (1 equiv.) at ambient temp.; stirred for 15 min; not isolated; detd. by (1)H and (31)P NMR spectroscopy;
参考文献
Beachley Jr.; Chao, Sun-Hua L.; Churchill, Melvyn Rowen; Lake, Charles H.
Organometallics, 2001 , vol. 20, # 23 p. 4896 - 4902
in hexane phosphine (2 equiv.) added dropwise at -78°C to Fe complex suspn., stirred for 30 min, warmed slowly to 20°C; hydrolyzed (H2O), org. layer sepd., dried (Na2SO4), solvent removed (vac.), crystd. at 5°C for hours; elem. anal.;
1: AdCH2Br With magnesium in diethyl ether 0.666667 h; CoolingInert atmosphere; 2: bis-isopropylchlorophosphine in diethyl ether T=-78 - 20°C; 8 h; Inert atmosphere;
参考文献
Millard, Matthew D.; Moore, Curtis E.; Rheingold, Arnold L.; Figueroa, Joshua S.
Journal of the American Chemical Society, 2010 , vol. 132, # 26 p. 8921 - 8923
1: bis-isopropylchlorophosphine With lithium in tetrahydrofuran T=0 - 20°C; 72 h; 2: Cl(CH2)2N(TMS)2 in tetrahydrofuran T=0°C; 4 h; Heating / reflux; 3: With sodium hydroxide; sulfuric acid; water more than 3 stages;
参考文献
KANATA CHEMICAL TECHNOLOGIES INC.
Patent: WO2008/148202 A1, 2008 ;
Location in patent: Page/Page column 34 ;
lithium aluminium tetrahydride in diethyl ether T=20°C;
参考文献
Zhu, Keming; Achord, Patrick D.; Zhang, Xiawei; Krogh-Jespersen, Karsten; Goldman, Alan S.
Journal of the American Chemical Society, 2004 , vol. 126, # 40 p. 13044 - 13053
in neat (no solvent) under Ar, standard vac. line techniques; ClP(i-Pr)2 and In compd. (molarratio 1:1) combined; 1 d at 20°C; recrystd. from pentane at low temp.; detd. by (1)H and (31)P NMR spectroscopy;
参考文献
Beachley Jr.; Chao, Sun-Hua L.; Churchill, Melvyn Rowen; Lake, Charles H.
Organometallics, 2001 , vol. 20, # 23 p. 4896 - 4902
in benzene-d6 byproducts: P2(i-Pr)4; under Ar, standard vac. line techniques, in NMR tube; benzene-d6 soln. of ClP(i-Pr)2 and In compd. degassed at -196°C in vac.; ClP(i-Pr)2soln. poured onto In compd. (molar ratio 1:1); sealed under vac.; 30 mi n at room temp.; not isolated; detd. by (1)H and (31)P NMR spectroscopy;
参考文献
Beachley Jr.; Chao, Sun-Hua L.; Churchill, Melvyn Rowen; Lake, Charles H.
Organometallics, 2001 , vol. 20, # 23 p. 4896 - 4902
in benzene-d6 byproducts: (Me3CCH2)P(i-Pr)2; under Ar, standard vac. line techniques, in NMR tube; benzene-d6 soln. of ClP(i-Pr)2 added to soln. of In compd. (molar ratio 1:1); evacuated; degassed at -196°C in vac.; sealed; 1 d; not isolated; detd. by (1)H and (31)P NMR spectroscopy;
参考文献
Beachley Jr.; Chao, Sun-Hua L.; Churchill, Melvyn Rowen; Lake, Charles H.
Organometallics, 2001 , vol. 20, # 23 p. 4896 - 4902
