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Vidwans, D. H. (1962) Interaction of titanium halides with esters of phosphorus. Doctoral thesis, Northern Polytechnic.
Interaction of titanium tetrachloride with dialkyl hydrogen phosphites (Alkyl = Et, Prⁿ, Prⁱ, Buⁿ, Buⁱ) and trialkyl phosphates, (Alkyl = Et, Buⁿ, Buⁱ) first involves the formation of a complex (RO₂P = 2P = OH.TiCl₄; (RO)₃P = O.TiCl₄ ; at temperatures below 0°, and then elimination of alkyl chloride and hydrogen chloride, and formation of a network of—P — 0 — Ti — 0 — links giving substances in the range Ti₂P₂0₉ — Ti₄P₄O₁₆. The elimination occurred approximately stepwise as the temperature was raised by the following stages: -100° (2 hr.) and 200° (2 hr.) and finally the residue was heated in an open crucible to about 10000°. Most of the elimination of chlorine and alkyl group occurred during the first stage of heating. During the second stage of heating s-butyl chloride was formed from the n-butyl esters and t-butyl chloride was formed from the isobutyl esters. Diphenyl hydrogen phosphite reacted with titanium tetrachloride to give hydrogen chloride and trichlorotityl- diphenyl phosphite (PhO)₂ PH0+ TiCl₄ → HC1 + (Ph0) ₂P0TiCl₃. Titanium tetrachloride and triphenyl phosphate formed 1:1 and 1:2 co-ordination compounds and there was no elimination of chlorobenzene.
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