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Purification of Laboratory Chemicals, 8th Edition by W.L.F. Armarego

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cis-cis-cis-1,2,3,4-Tetrakis(diphenylphosphinomethyl)cyclopentane [(1R*,2R*,3S*,4S*)-tetrakis-(diphenylphosphinomethyl)cyclopentane, Tedicyp] [333380-86-2] C57H54P4, M 862.9, m 79°. The intermediate cis-cis-cis-1,2,3,4-tetrakis(boranatodiphenylphosphanylmethyl)cyclopentane (white crystals m 149°, after chromatography on silica gel eluting with AcOEt/petroleum ether, 1:4) is obtained from Ph2PLi (from Ph2PCl see [1079-66-9] and Li) and cis-cis-cis-1,2,3,4-tetrakis(tosyloxymethyl)cyclopentane in THF under argon (~ 20°/5 hours), then borane in THF is added. This boranato intermediate formed is added to anhydrous Et2NH, heated at 55-60° for 10 hours, evaporated to dryness, this process is repeated twice, and the residue is chromatographed on silica ...

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