242132-31-6Relevant articles and documents
Synthesis of cyclenphosphoranes with polyfluorophenyl substituents; An X-ray structure of N-methyl cyclen-p-(heptafluorotolyl)phosphorane
Gupta,Kirchmeier, Robert L.,Shreeve, Jeanine M.
, p. 223 - 228 (1999)
The metathesis reactions between the lithiated derivative of cyclenphosphorane (2) and octafluorotoluene, hexafluorobenzene, pentafluorobenzonitrile, pentafluoronitrobenzene, pentafluoro-n-butylbenzene, pentafluorobenzene and p-(cyanotetrafluorophenoxy-pentafluorobenzene) under reflux conditions gave cyclen-p-(heptafluorotolyl)phosphorane (3), cyclen-p-(pentafluorophenyl)phosphorane (4), cyclen-p-(cyanotetrafluorophenyl)phosphorane (5), cyclen-p-(tetrafluoronitrophenyl)phosphorane (6), cyclen-p-(n-butyltetrafluorophenyl)phosphorane (7), cyclen-p-(tetrafluorophenyl)phosphorane (8) and cyclen-p-(p-cyanotetrafluoro-phenoxytetrafluorophenyl)phosphorane (9), respectively, in good yields. All products were characterized by spectral and analytical techniques. These materials are moderately stable thermally but are moisture sensitive, hydrolyzing to form cyclen phosphine oxide (10). Addition of CH3I to 3 affords the phosphoammonium iodide (11). The X-ray crystal structure of 11 was obtained. The crystal is triclinic with a space group P1. The unit cell parameters a=7.8652(2) A, b=8.584(2) A, c=22.1573(3) A; α=80.9010(10)°; β=79.2490(10)°; γ=76.9930(10)°; and Z=2.