| Autor: |
Srinivas, Bhamidi, Chang, Chung-Cheng, Chen, Chau-Han, Y. Chiang, Michael, Chen, I.-Ting, Wang, Yu, Lee, Gene-Hsiang |
| Zdroj: |
Journal of the Chemical Society, Dalton Transactions; January 1997, Vol. 1997 Issue: 6 p957-964, 8p |
| Abstrakt: |
A series of magnesium–isothiocyanate and –carbodiimide insertion products, Mg(SCPhNBut)2(thf)21, Mg(SCPhNPh)2(thf)22, Mg(PriNCRNPri)2(thf)2 (R = Ph 3, Et 4 or Pri5) and Mg(ButNCEtNBut)2(thf)26 have been prepared by the stoichiometric reaction between MgR2 (R = Ph, Et or Pri) and various isothiocyanates and carbodiimides in tetrahydrofuran (thf) solution. The 1∶1 reaction between bis(diisopropylamido)magnesium and 1,3-diisopropylcarbodiimide gave a dinuclear complex Mg2(-NPri2)2[(Pri N)2CNPri2]27 and a mononuclear complex Mg[(PriN)2CNPri2]2 (thf) 8 when the stoichiometry is 1∶2. The mononuclear complexes Mg[SC(NPh)NR2]2(thf)2 (R = Pri9 or Et 10) were obtained using phenyl isothiocyanate and bis(diethylamido)- or bis(diisopropylamido)-magnesium in 1∶1 stoichiometric ratio. A plausible mechanism for the formation of 7 and 8 is suggested. Reaction between MgEtBr and PhNCS in diethyl ether gave the dinuclear complex Mg2(SCEtNPh)4(OEt2)211. All of the complexes were characterized by 1H, 13C NMR and IR spectroscopy as well as elemental analysis. The crystal structures of 1, 3, 8, 9 and 11 were determined by single-crystal X-ray diffraction. The reaction of complex 1 with an excess of PhNCO resulted in the cyclotrimerization of phenyl isocyanate to give (PhNCO)3·thf. |
| Databáze: |
Supplemental Index |
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