NaOH in toluene byproducts: H2; N2 atmospher; treatment of catechol and NaOH in toluene (stirring, 30 min), dropwise addn. of GaI in toluene (4 h); sepn. of NaI (filtration off, drying), collectin of Ga-complex by evapn. of filtrate;
参考文献
Ozarowski, Andrzej; McGarvey, Bruce R.; El-Hadad, Ahmed; Tian, Zhigang; Tuck, Dennis G.; et al.
Inorganic Chemistry, 1993 , vol. 32, p. 841 - 847
C2H4(P(C6H5)2)2 in tetrahydrofuran; toluene byproducts: C5H5N, CO, H2; Treating of suspn. of diphos and (H-py)I in THF with Nb-complex at room temp. under a CO atmosphere.; Immediate react. with evolution of CO and H2 (gas chromy.) obsd. Stirring (2 h, room temp.), removal of THF (vac., room temp.), dissolving of residue (toluene, CO), stirring (2 h), filtn., treating with n-heptane. Sepn. of microcryst., elem. anal.;
C2H4(P(C6H5)2)2 in tetrahydrofuran; toluene byproducts: C5H5N, CO, H2; Treating of suspn. of diphos and (H-py)I in THF with Ta-complex at room temp. under a CO atmosphere.; Immediate react. with evolution of CO and H2 (gas chromy.) obsd. Stirring (2 h, room temp.), removal of THF (vac., room temp.), dissolving of residue (toluene, CO), stirring (2 h), filtn., treating with n-heptane. Sepn. of microcryst., elem. anal.;
C2H4(P(C6H5)2)2; I2 in tetrahydrofuran; toluene byproducts: CO; Treating of suspn. of starting compd. in THF with I2 (-78°C, N2 or Ar). Evolution of gas and formation of red soln. takes place upon mixing. Addn. of diphos at -50°C, stirring (room temp.).; Removal of solvent (vac.), dissolving of residue in toluene, filtn., treatment with n-heptane, cooling (-30°C), elem. anal.;
C2H4(P(C6H5)2)2; I2 in tetrahydrofuran; toluene byproducts: CO; Treating of suspn. of starting compd. in THF with I2 (-78°C, N2 or Ar). Evolution of gas and formation of red soln. takes place upon mixing. Addn. of diphos at -50°C, stirring (1 h, room temp.).; Removal of solvent (vac.), dissolving of brown residue in toluene, filtn., treatment with n-heptane, cooling (-30°C), elem. anal.;
