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[摘要]：The reaction of tetrachlorodiphosphines [Cl2P(CH2)nPCl2; n = 2-4] with fluorous arom. precursors 4-bromo(perfluorohexyl)benzene and 4-(perfluorohexyl)phenol gave a series of fluorous-tagged diphosphines [(p-C6F13C6H4)2P(CH2)nP(C6H4C6F13-p)2; n = 2-4] and a new diphosphonite [(p-C6F13C6H4O)2P(CH2)3P(OC6H4C6F13-p)2]. The improved synthesis of 1,3-bis(dichlorophosphino)propane (dcpp), involved the facile chlorination of the corresponding primary phosphine with triphosgene. Fluorinated diimines RN:C(CH3)C(CH3):NR, where R = p-C6H4C6F13 or p-C6H4C8F17 have also been prepd., and were air-stable alternatives to the highly air-sensitive phosphorus-contg. ligands. All compds. were characterized by a variety of techniques including NMR, IR, MS and microanal. The successful redn. of the phosphine-oxides [(p-C6F13C6H4)2P(O)(CH2)nP(O)(C6H4C6F13-p)2; n = 2,3] with phenylsilane is also presented. |
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