in dichloromethane
byproducts: N2; condensation excess HBr onto bis(dinitrogen) complex at -196°C; evolution of 1 mol N2; addn. of CH2Cl2; 60 h;; monitoring by (31)P-NMR;;
参考文献
Baumann, John A.; Bossard, Gerald E.; George, T. Adrian; Howell, Daniel B.; Koczon, Lenore M.; et al.
Inorganic Chemistry, 1985 , vol. 24, p. 3568 - 3578
KOH in hydrogen bromide
aq. HBr; condensing propylene carbonate onto Mo-complex (-196°C), warming to 20°C, addn. of excess aq. HBr, stirring for 48 h, addn. of excess 40percent KOH; distn. into dild. H2SO4, colorimetry of NH3 and N2H4, volumetry of free and total N2 (after reaction with NaOBr);
参考文献
Chatt, Joseph; Pearman, Alan J.; Richards, Raymond L.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1977 , p. 1852 - 1860
in tetrahydrofuran
byproducts: N2, NH4Br, P(C6H5)3; cooling bis(dinitrogen) complex in round-bottom flask to -196°C;distilling HBr into flask (ratio HBr:Mo=15:1 or 6:1), increment addn.; addn. of THF; evacn.; warming to room temp., evolution of gas at about 0°C; 68 h;; monitoring by (31)P-NMR;;
参考文献
Baumann, John A.; Bossard, Gerald E.; George, T. Adrian; Howell, Daniel B.; Koczon, Lenore M.; et al.
Inorganic Chemistry, 1985 , vol. 24, p. 3568 - 3578
in tetrahydrofuran
byproducts: N2, NH4Br, P(C6H5)3; cooling bis(dinitrogen) complex in round-bottom flask to -196°C;distilling HBr into flask (ratio HBr:Mo=19:1); addn. of THF; evacn.; warming to room temp., evolution of gas at about 0°C, 62 h;; monitoring by (31)P-NMR; isolation of Mo compound: vac. distn.; addn. of methanol to oily residue, stirring several hours; filtration; drying;;
参考文献
Baumann, John A.; Bossard, Gerald E.; George, T. Adrian; Howell, Daniel B.; Koczon, Lenore M.; et al.
Inorganic Chemistry, 1985 , vol. 24, p. 3568 - 3578
→
反应条件
in benzene
byproducts: N2; condensation excess HBr onto bis(dinitrogen) complex at -196°C; evolution of 1 mol N2; addn. of benzene; warming up or removal of volatiles, addn. of CH2Cl2 and stirring for different time;; monitoring by (31)P-NMR;;
参考文献
Baumann, John A.; Bossard, Gerald E.; George, T. Adrian; Howell, Daniel B.; Koczon, Lenore M.; et al.
Inorganic Chemistry, 1985 , vol. 24, p. 3568 - 3578
in neat (no solvent)
N2-atmosphere; condensation of HBr at -196°C onto V-complex (54percent purity; prepd. from VCl3(THF)3, Na and phosphine ligand by pptn. with pentane and drying), slow warming to room temp. with stirring, evapn., drying (high vac.), addn. of aq. NaOH;
参考文献
Gailus, Hartmut; Woitha, Claus; Rehder, Dieter
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1994 , # 23 p. 3471 - 3478
