On the preparation of tetramethylammonium trifluoromethylbistrifluoromethylnitroxyliodate(I) (CH3)(4)N+(CF3)2NOICF(3)(-) and the reaction of tetramethylammonium bistrifluoromethylnitrate (CH3)(4)N+(CF3)(2)NO- with Cl-2 and ClONO2

The preparation of (CF3)(2)NO- as tetramethylammoniumsalt and its addition reaction with CF3I are described. The formed Tetramethylammonium trifluoromethylbistrifluoromethylnitroxyliodate(I) (CH3)(4)N+(CF3)(2)NOICF3- is characterized by its spectra and the reaction with CF3OCl. In addition we present our approach to the preparation of (CF3)(2)NOCl by the reaction of (CH3)(4)N+(CF3)(2)NO- With Cl-2 and ClONO2. The thermolabile compounds have been characterized by i. r., Raman, F-19 and C-13 NMR spectra.