hydrogen in neat (no solvent) dry solvents; degassing Mo-compd. dissolved in EtCN, placing under hydrogen (400 Torr at -196°C), stirring react. mixt. at room temperature (1 day); removal of solvent under reduced pressure, extn. (water), dissolving in MeCN, pptn. by addn. of Et2O; elem. anal.;
hydrogen in acetonitrile dry solvents; degassing Mo-compd. dissolved in acetonitrile, placing under hydrogen (400 Torr at -196°C), stirring react. mixt. at room temperature (1 day); removal of solvent under reduced pressure, extn. (water), dissolving in MeCN, pptn. by addn. of Et2O;
hydrogen in benzonitrile dry solvents; degassing Mo-compd. dissolved in PhCN, placing under hydrogen (400 Torr at -196°C), stirring react. mixt. at room temperature (1 day); removal of solvent under reduced pressure, extn. (water), , dissolving in MeCN, pptn. by addn. of Et2O;
N,N-methylenediacrylamide; Cu(BF4)2*6H2O in water; dimethyl sulfoxide byproducts: 2-MeC6H4CH2CH(SCN)CONHCH2NHCOCHCH2; addn. of 2-MeC6H4N2BF4 (1.1 equiv.) to N,N-methylenediacrylamide (1 equiv.), Cu(BF4)2*6H2O (0.1 equiv.) and NH4SCN (1.1 equiv.) in H2O-DMSO (1:4) for 30 min; evolution of gas at 10-15°C for 45 min;
参考文献
Russian Journal of General Chemistry, , vol. 73, # 6 p. 957 - 960
N,N-methylenediacrylamide; Cu(BF4)2*6H2O in water; dimethyl sulfoxide byproducts: 2,5-Cl2C6H3CH2CH(SCN)CONHCH2NHCOCHCH2; addn. of 2,5-Cl2C6H3N2BF4 (1.1 equiv.) to N,N-methylenediacrylamide (1 equiv.) , Cu(BF4)2*6H2O (0.1 equiv.) and NH4SCN (1.1 equiv.) in H2O-DMSO (1:4) for 30 min; evolution of gas at 10-15°C for 45 min;
参考文献
Russian Journal of General Chemistry, , vol. 73, # 6 p. 957 - 960
N,N-methylenediacrylamide; Cu(BF4)2*6H2O in water; dimethyl sulfoxide byproducts: 4-MeOC6H4CH2CH(SCN)CONHCH2NHCOCHCH2; addn. of 4-MeOC6H4N2BF4 (1.1 equiv.) to N,N-methylenediacrylamide (1 equiv.), Cu(BF4)2*6H2O (0.1 equiv.) and NH4SCN (1.1 equiv.) in H2O-DMSO (1:4) for 30 min; evolution of gas at 10-15°C for 45 min;
参考文献
Russian Journal of General Chemistry, , vol. 73, # 6 p. 957 - 960
N,N-methylenediacrylamide; Cu(BF4)2*6H2O in water; dimethyl sulfoxide byproducts: C6H5CH2CH(SCN)CONHCH2NHCOCHCH2; addn. of PhN2BF4 (1.1 equiv.) to N,N-methylenediacrylamide (1 equiv.), Cu(BF4)2*6H2O (0.1 equiv.) and NH4SCN (1.1 equiv.) in H2O-DMSO (1:4) for 30 min; evolution of gas at 10-15°C for 45 min;
参考文献
Russian Journal of General Chemistry, , vol. 73, # 6 p. 957 - 960