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- W1992912171 abstract "The bulky primary phosphane 2,6-diisopropylphenylphosphane, DipPH 2 , has been prepared from 1-bromo-2,6-diisopropylbenzene via the reaction of the Grignard reagent with PCl 3 . The resulting mixed phosphonous dihalides DipP(Cl,Br) 2 are reduced with LiAlH 4 to yield the title compound in reasonable yield and on a synthetically useful scale. DipPH 2 is also used to prepare the monosilylated derivatives DipPHSi(CH 3 ) 3 and DipPH{Si(CH 3 ) 2 -t-Bu} as well as the disilylated compounds DipP{Si(CH 3 ) 3 } 2 and DipP{Si(CH 3 ) 2 -t-Bu} 2 . All products have been fully characterized by IR, mass, and NMR spectroscopy. The crystal structure of DipPH{Si(CH 3 ) 2 -t-Bu} was determined from single-crystal diffraction data: C 18 H 33 PSi, P2 1 /c, Z = 4, a = 8.5768(10), b = 28.104(3), c = 8.1102(4) Å, β = 93.341(3)° (R = 0.0518). Changes in the NMR spectrum of DipPH{Si(CH 3 ) 2 -t-Bu} were observed over the temperature range 178380 K. Barrier heights were determined from the peak separation at low temperature and the coalescence points: ΔG [Formula: see text] 40 kJ mol 1 for C(aryl)P bond rotation and [Formula: see text] 72 kJ mol 1 for pyramidal inversion at phosphorus.Key words: crystal structure, 2,6-diisopropylphenyl, bulky substituents, steric congestion, dynamic NMR, primary phosphane, silyl phosphane." @default.
- W1992912171 created "2016-06-24" @default.
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- W1992912171 date "2002-11-01" @default.
- W1992912171 modified "2023-10-03" @default.
- W1992912171 title "2,6-Diisopropylphenylphosphane: A new, bulky primary phosphane and its mono- and disilylated Si(CH<sub>3</sub>)<sub>3</sub> and Si(CH<sub>3</sub>)<sub>2</sub>-<i>t</i>-Bu derivatives A synthetic, crystallographic, and dynamic NMR investigation" @default.
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- W1992912171 doi "https://doi.org/10.1139/v02-150" @default.
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