References
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- Hirschmann , R. , Yager , K. M. , Taylor , C. M. , Moore , W. , Sprengeler , P. A. , Witherington , J. , Phillips , B. W. and Smith , A. B. III . 1995 . J. Am. Chem. Soc. , 117 : 6370
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- Quin , L. D. and Jankowski , S. unpublished results
- 34P NMR spectra were recorded on a Broker 80 MHz Spectrometer, with 85% phosphoric acid as reference. Downfield shifts are positive. 1H NMR spectra were recorded on the same instrument. Phenylphosphonic dichloride was purchased from Aldrich Chemical Co.; it must be redistilled with fractionation before use, as it contains a significant amount of phenylphosphonous dichloride (lower boiling) that will interfere with later reactions. The fractionation is easily monitored by 31P NMR: PhPOC12, Δ 31.6; PhPCI2, Δ 160.6. All solvents were carefully dried and distilled before use, and apparatus was generally flame-dried. Reactions were conducted under argon