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

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Phenylphosphonous dichloride (P,P-dichloro phenyl phosphine) [644-97-3] C6H5Cl2P, M 179.0, has m -51°, b 68-70°/1mm, 224-226°/atm, d430 1.9317, nD35 1.5962. Distil it in a vacuum by fractionating through a 20cm column packed with glass helices (better to use a spinning band column) [Buchner & Lockhart J Am Chem Soc 73 755 1951, DOI: 10.1021/ja01146a076; NMR: Muller et al. J Am Chem Soc 78 3557 1956, DOI: 10.1021/ja01596a002; IR: Daasch & Smith Anal Chem 23 853 1951, DOI: 10.1021/ac60054a008]. It forms a yellow Ni complex: Ni(C6H5Cl2P)4 (m 91-92°, from H2O) [Quin J Am Chem Soc 79 3681 1957, DOI: 10.1021/ja01571a020], and a yellow complex also with molybdenum carbonyl: Mo(CO)3.(C6H5Cl2P)3 (m 106-110° dec) [Abel et al. J Chem Soc 2323 1959, DOI: ...

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