chloro(trifluoro)methane

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a 2.03 mmol sample of CF3CO2Cl contained in a U-trap at -78°, hexafluoropropylene (2.72 mmol) was slowly added. After several hours the mixture was warmed to ambient temperature for 1 hour prior to fractional condensation through traps cooled to -78° and -196°. The -196° fraction consisted of one mmol C3F3 and 0.27 mmol each of CF3Cl and CO2. The material retained at -78° was a colorless liquid and was identified as CF3CO2CF2CFClCF3 (1.70 mmol, 84% yield) on the basis of its vapor density molecular weight (297 found vs. 298.5 g/mol calculated), and controlled hydrolysis to a 1:1 mixture of CF3CFClCFO and CF3CO2H. Its spectroscopic properties confirmed this identification: infrared, cm-1 ; 1856(S), 1335(M), 1297(S), 1249(VS), 1205(S), 1137(S), 1088(VS), 970(S), 850(W), 740(W), 671(MW): mass spectrum, 40 ev; m/e (assign., rel. intens.) 298(M, 0.01), 279(M--F, 0.03), 263(M--Cl, 0.03), U-trap at -78° to fractional condensation through traps cooled to -78° and -196° The -196° fraction retained at -78°