PREPARATION AND SINGLE-CRYSTAL X-RAY-DIFFRACTION STUDY OF SOME FLUOROPHOSPHITES AND PHOSPHITE ESTERS

The synthesis of some monofluorophosphite esters from the appropriate hydroxy compound and PCl2F in the presence of a tertiary amine is desc ribed. The reaction of 2,2'-dihydroxy-biphenyl with PCl3 in the presen ce of triethylamine did not furnish the expected chlorophosphite 9; in stead, the bridged bisphosphite ester, 10, was obtained. Reaction of t he fluorophosphite ester 8 with 3,5-di-tert-butyl-benzoquinone furnish ed the spiromonofluorophosphorane 12 in which lambda5P is part of a fi ve-membered and a seven-membered ring system. Single crystal X-ray dif fraction studies were conducted on compounds 2, 10 and 13. In the case of 2, crystallographic 2/m symmetry and short intermolecular P...O di stances were observed. Compound 10 shows short intramolecular P...O co ntacts. The catechyl phosphate 13, similarly to other dialkylphosphate esters, was found to be a hydrogen-bonded dimer.