ChemInform Abstract: N‐CHLOR‐N‐TRIMETHYLSILYLACYLAMIDE

Abstract

Aus äquimolaren Mengen von N,N‐Dichloracylamiden (I) und Trimethyl‐dialkylaminosilanen (II) werden in Tetrachlorkohlenstoff die Verbindungen (III) in 55‐65%iger Ausbeute erhalten.

“Living” Cationic Polymerization of Phosphoranimines as an Ambient Temperature Route to Polyphosphazenes with Controlled Molecular Weights

“…Multiple distillations did not remove (Me 3 Si) 2 NCl because this compound distills at a similar temperature and pressure to 1 . Pure 1 was obtained by treatment of the mixture with PPh 3 (in an excess or stoichiometric amount relative to (Me 3 Si) 2 NCl) in CH 2 Cl 2 to form Ph 3 PNSiMe 3 and Me 3 SiCl . The resultant mixture was then distilled at reduced pressure to yield pure 1 .…”

“…Pure 1 was obtained by treatment of the mixture with PPh 3 (in an excess or stoichiometric amount relative to (Me 3 Si) 2 NCl) in CH 2 Cl 2 to form Ph 3 PdNSiMe 3 and Me 3 SiCl. 13 The resultant mixture was then distilled at reduced pressure to yield pure 1. Alternatively, to avoid the additional purification step, 1 has also been obtained from the reaction of PCl 5 with N(SiMe 3 ) 3 in hexane at -78 °C.…”

“…Equipment. 31 P, 13 C, and 1 H spectra were recorded with use of a Bruker WM-360 NMR operated at 146, 90.27, and 360 MHz, respectively. 29 Si NMR spectra were recorded with use of a Bruker AM-300 NMR operated at 59.6 MHz and were referenced externally to SiMe4.…”

“…29 Si NMR spectra were recorded with use of a Bruker AM-300 NMR operated at 59.6 MHz and were referenced externally to SiMe4. 1 H and 13 C NMR spectra are referenced to an internal CDCl3. 31 P NMR chemical shifts are relative to 85% phosphoric acid as an external reference, with positive shift values downfield from the reference.…”

“…1 H NMR (CDCl3): δ ) 0.18 ppm (d, 4 JPH ) 1 Hz); 31 P NMR (CDCl3): δ ) -54 ppm. 13 C NMR (CDCl3): 1.9 ppm (d, 4 JCP 7 Hz, SiCH3); 29 Si NMR (CDCl3): δ ) 0.27 (d, 2 JPSi ) 11 Hz). MS (CI, isobutane): m/z ) 224 (MH + , 98), 208 (M + -Me, 82), in good agreement with isotopic abundance calculations.…”