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However, the authors observed significant oxidation of the phosphine end groups during its isolation which they did not isolate in pure form
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A recent report attempts the synthesis of 2 for use as a macroinitiator in block copolymer synthesis (Choi, Y. K.; Bae, Y. H.; Kim, S. W. Macromolecules 1995, 28, 8419-8421). However, the authors observed significant oxidation of the phosphine end groups during its isolation which they did not isolate in pure form.
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However, in our hands the obtained yields were even lower (38%). Therefore, we adopted a three-step approach to 5, with the overall yield being 85% (Scheme 1)
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A recent report descibes a one-step route to phosphine 5 in moderate yield (63% yield) [Herd, H.; Hessler, A.; Hingst, W.; Tepper, M.; Stelzer, O. J. Organomet. Chem. 1996, 522, 69-76]. However, in our hands the obtained yields were even lower (38%). Therefore, we adopted a three-step approach to 5, with the overall yield being 85% (Scheme 1).
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