GLC study of redistribution reactions of radicals in organotin monohalide series

Author(s):  
V. A. Chernoplekova ◽  
N. N. Zemlyanskii ◽  
N. D. Kolosova ◽  
K. A. Kocheshkov
1992 ◽  
Vol 30 (4) ◽  
pp. 613-623 ◽  
Author(s):  
V. Belot ◽  
R. J. P. Corriu ◽  
D. Leclercq ◽  
P. H. Mutin ◽  
A. Vioux

2009 ◽  
Vol 87 (8) ◽  
pp. 1163-1172 ◽  
Author(s):  
Osamah Alhomaidan ◽  
Gregory C. Welch ◽  
Guangcai Bai ◽  
Douglas W. Stephan

A series of phosphinimide complexes of Hf are prepared and characterized. Reaction of the phosphinimine t-Bu3PNH with Hf(NEt2)4 gave (t-Bu3PN)Hf(NEt2)3 (1) but this species was not readily converted to the corresponding HfCl3-derivative. The reaction of 2 equiv. of t-Bu3PNH with Hf(NEt2)4, however, gave (t-Bu3PN)2Hf(NEt2)2 (2), which was readily converted to (t-Bu3PN)2HfCl2 (3) and (t-Bu3PN)2HfMe2 (4). Employing t-Bu3PNLi and HfCl4 afforded (t-Bu3PN)3HfCl (5) while reaction with CpHfCl3 gave rise to ligand redistribution reactions affording (t-Bu3PN)2HfCl2 and Cp2HfCl2. However, Cp(t-Bu3PN)2HfCl (7) was prepared by treating (t-Bu3PN)2HfCl2 with CpNa. The related species of Cp2(t-Bu3PN)HfCl (8) was synthesized by the reaction of Cp2HfCl2 and t-Bu3PNLi. Ligand redistribution was avoided in the reaction of Cp*HfCl3 as Cp*(t-Bu3PN)HfCl2 (9) and Cp*(i-Pr3PN)HfCl2 (10) were readily obtained and derivatized as Cp*(t-Bu3PN)Hf(NMe2)2 (11) and Cp*(t-Bu3PN)HfMe2 (12), respectively. Similarly, ((Me3Si)2C5H3)(t-Bu3PN)HfCl2 (13) was converted to ((Me3Si)2C5H3)(t-Bu3PN)HfMe2 (14). Reactions with Lewis acid activators were used to prepare Cp*(t-Bu3PN)HfMe(THF)MeB(C6F5)3 (15), (Cp*(t-Bu3PN)HfMe)(B(C6F5)4) (16), and (t-Bu3PN)2Hf(H2B(C6F5)2)2 (17). Preliminary testing of 3, 9, and 13 in ethylene polymerization is reported. Compounds 3, 4, 7, 9, and 17 are characterized crystallographically.


1976 ◽  
Vol 54 (13) ◽  
pp. 2135-2140 ◽  
Author(s):  
J. Dazord ◽  
H. Mongeot ◽  
H. Atchekzai ◽  
J. P. Tuchagues

The mixed halide–pseudohalides BXn(NCS)3−n (n = 1 or 2) have been obtained except for X = F. Mixtures of these compounds with boron trihalide and boron triisothiocyanate are prepared by the reaction of BX3 either with metal isothiocyanates or with boron triisothiocyanate. Mass spectrometry, infrared, Raman, and 11B nmr data are reported. Rapid redistribution reactions prevent the isolation of the mixed species. Vibration spectrometry shows that boron is bonded to the nitrogen of the NCS group and not to the sulfur.


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