triphenylphosphine in acetonitrile under N2, addn. of TMNO dihydrate to carbonyl-compd. in CH3CN at 0°C, addn. of PPh3 after stirring for 10 min, stirred for 16 h at 0°C; evapn. under vac., filtration, recrystn. (CH2Cl2/CH3OH or CH2Cl2/hexane); elem. anal.;
参考文献
Hor, T. S. Andy
Inorganica Chimica Acta, 1988 , vol. 143, p. 3 - 6
in acetonitrile Preparation under dry nitrogen; Cr(CO)6 and TMNO were added to acetonitrile giving a yellow solution; PPh3 was added, stirring at room temperature for 16h; filtration; filtrate was cooled at -20°C; recrystallization in CHCl3/EtOH; DSC, TG, elem. anal.;
参考文献
Hor, T. S. Andy; Chan, Hardy S. O.; Chiam, Caroline S. M.; Lim, Kok Hwa
Thermochimica Acta, 1988 , vol. 128, p. 175 - 184
in tetrahydrofuran; dichloromethane under N2; ratio of Mo(CO)6:dppf:TMNO = 1:0.4:0.8; using TMNO as an initiator; stirred at 28°C for 3.5 h; removal solvents in vacuo; residue extracted with CH2Cl2; soln. applied to silica TLC; elution with 20percent CH2Cl2 in hexane; recrystn. from CH2Cl2/hexane; elem. anal.;
参考文献
Journal of Organometallic Chemistry, , vol. 373, p. 319 - 324
pyridine in tetrahydrofuran
under N2, addn. of TMNO dihydrate to carbonyl-compd. in THF at 28°C, addn. of pyridine after stirring for 10 min, stirred for 3 h at 28°C; evapn. under vac., filtration, recrystn. (CH2Cl2/CH3OH or CH2Cl2/hexane); elem. anal.;
参考文献
Hor, T. S. Andy
Inorganica Chimica Acta, 1988 , vol. 143, p. 3 - 6
triphenylphosphine in acetonitrile
under N2, addn. of TMNO dihydrate to carbonyl-compd. in CH3CN at 0°C, addn. of PPh3 after stirring for 10 min, stirred for 16 h at 0°C; evapn. under vac., filtration, recrystn. (CH2Cl2/CH3OH or CH2Cl2/hexane); elem. anal.;
参考文献
Hor, T. S. Andy
Inorganica Chimica Acta, 1988 , vol. 143, p. 3 - 6
in acetonitrile
preparation under dry nitrogen; Mo(CO)6 and TMNO were added to acetonitrle giving a yellow solution; PPh3 was added to the mixture; stirring for 16h at room temperature; filtration; filtrate was cooled at -20°C; recrystallization in CHCl3/EtOH; TA, elem. anal.;
参考文献
Hor, T. S. Andy; Chan, Hardy S. O.; Chiam, Caroline S. M.; Lim, Kok Hwa
Thermochimica Acta, 1988 , vol. 128, p. 175 - 184