A convenient synthesis of carbonyl chloride fluoride

Existence of the Halocarbonyl and Trifluoromethyl Cations in the Condensed Phase

“… A detailed investigation of these adducts is given elsewhere . On thermal decomposition of the solid Cl 2 CO·SbF 5 adduct or in SO 2 ClF solution at −78 °C, a quantitative chlorine−fluorine exchange of one of the two chlorine ligands of Cl 2 CO was observed (eq 3) …”

“…Commercially available phosgene (Matheson), F 2 CO (PCR Research Chemicals), AsF 5 , and SbF 5 (Ozark Mahoning) were purified by fractional condensation prior to use. Literature methods were used for the syntheses of ClFCO, Cl 2 CO·SbF 5 , and tert -butyl fluoroformate …”

“…Commercially available phosgene (Matheson), F2CO (PCR Research Chemicals), AsF5, and SbF5 (Ozark Mahoning) were purified by fractional condensation prior to use. Literature methods were used for the syntheses of ClFCO, 13 Cl2CO‚ SbF5, 14 and tert-butyl fluoroformate. 15 Volatile materials were handled in a stainless steel vacuum line equipped with Teflon-FEP U-traps, stainless steel bellows-seal valves, and a Heise Bourdon tube-type pressure gauge.…”

Experimental and Theoretical Characterization of the Oxygen-Coordinated Donor−Acceptor Adducts of COCl2, COClF, and COF2with AsF5and SbF5

“… The 1:1 compositions were established by the observed material balances and for the COF 2 /AsF 5 system by a tensimetric titration (vapor pressure−composition isotherm) 4 at −78 °C which gave evidence only for a 1:1 adduct. The resulting adducts are white solids which are thermally unstable and decompose reversibly to the starting materials, except for the COCl 2 /SbF 5 system for which rapid irreversible fluorine−chlorine exchange is observed (eq 2) The oxygen-bridged nature of these adducts was established by vibrational and multinuclear NMR spectroscopy and the results from the theoretical calculations.…”

“…Antimony pentafluoride (Ozark Mahoning) was distilled prior to use. The COClF was prepared by a literature method …”